CARBORUNDUM UNIVERSAL LIMITED

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1 MagAl Spinel Zirconia Vs. Alumina - Zirconia Refractory for Hard Black Reactor Ravikumar N, Ranjan Dey, Eswaran V T, Rajagopalan R CARBORUNDUM UNIVERSAL LIMITED

2 Contents : Refractory Application in Carbon Black Reactor Issues in Hard Black Reactor Issues in Soft Black Reactor Addressing the issues w.r.t hot face refractory Study on Alumina Zirconia and Spinel Zirconia Composite Conclusion & Recommendation Product recommendation for various application areas Installation Service

3 Refractory Application in Carbon Black Reactor Hard Black Reactor Soft Black Reactor Inlet Box Drier Combustor Rotary Drier

4 Exposure on Refractories in Hard Black Reactor Extreme Temperature Thermal spalling Higher refractory wear in the restriction zone Temperature fluctuations due to grade changes Reaction between refractory and impurities in CBFS and with Chemical Additives Exposure on Refractories in Soft Black Reactor High Temperature Thermal spalling Reaction between refractory and impurities in CBFS and with Chemical Additives Localised combustion Localised heating due to improper burner alignment

5 Different Refractory Materials used for Venturi in Hard Black Reactors Alumina - Zirconia 99.5% Alumina Alumina- Chrome Zirconia MagAl Spinel - Zirconia

6 Issues towards Hot Face Refractory. Operating temperatures in hard black reactors are going beyond 1900 Deg.C to improve the operating efficiencies. We developed Alumina Zirconia composite for evaluating at high temperature applications. Which is proven to be good upto 1850 Deg.C. Presently, we are evaluating Mag Al Spinel + Zirconia composite as a next level to Alumina Zirconia Composite.

7 Study on Alumina Zirconia and Spinel Zirconia Composite

8 Comparison of Phase Diagram : Alumina Silica Vs Magnesia - Alumina Alumina Silica Phase Diagram Alumina Magnesia Phase Diagram

9 Two types of samples were taken for the study. Alumina Zirconia and Spinel Zirconia Composite Sample # Description Raw Material Base Firing Temperature Sample A 95% Alumina Alumina + Zirconia 1750 o C Sample B 25% MgO Spinel Spinel + Zirconia 1750 o C

10 Sample A: Alumina Zirconia Composite Sample B: Spinel Zirconia Composite

11 Tests carried out : Thermal Shock Resistance [TSR] to determine the effect of repeated heating and cooling. Pyrometric Cone Equivalent : To Determine the refractoriness Scanning Electron Microscopy [SEM] EDAX Analysis: To identify the phase morphology

12 Results of Thermal Shock Resistance [TSR] at 1000 Deg C Sample # Air Quenching (Cycle) Water Quenching (Cycle) Sample A Sample B

13 Results of Pyrometric Cone Equivalent Orton Cone 38 Sample B Sample A

14 Scanning Electron Microscopy [SEM] Sample A Homogeneous distribution of Zirconia in Matrix

15 Scanning Electron Microscopy [SEM] Sample B

16 OKa Counts Scanning Electron Microscopy [SEM] EDAX Analaysis Sample B MgKa AlKa mm kev

17 Counts OKa Scanning Electron Microscopy [SEM] EDAX Analaysis Sample B MgKa AlKa ZrLl ZrLa mm kev

18 High Resolution Optical Micrography Sample B Zirconia Particle Distribution in matrix

19 Inference of the Study From the Scanning Electron Microscopy [SEM] study, Uniform Zirconia distribution in matrix in sample A. SEM EDAX study on Spinel Zirconia, Observed uniform distribution of zirconia in matrix in Sample B. Both Alumina Zirconia and Spinel Zirconia refractoriness observed to be Orton Cone 38+. At present we are unable to do refractoriness test at 2000 Deg.C. In future, we are planning to do refractoriness test at 2000 Deg.C for both Sample A and Sample B. Thermal Shock Resistance of Spinel Zirconia observed to be superior when compared with Alumina Zirconia.

20 Conclusion From the study, it is found that sample A [CUMILOX 95AZ SPL] is more stable & suitable product for the severe application as hot face refractory in hard black reactor for application temperatures below 1850 Deg.C Sample B ( CUMILOX MA 26 ) to be analyzed for grain growth stability studies in repeated cycles at elevated temperature. Zirconia enhances the thermal shock resistance Observed Spinel based refractory possesses better thermal shock resistance compared to Alumina Zirconia.

21 Refractory Application in Hard Black Reactor (Typical Diagram)

22 Refractory Application in Hard Black Reactor Recommendation from CUMI APPLICATION AREA REFRACTORY HARD BLACK HIGH TEMPERATURE REACTOR TEMPERATURE 1700 o C o C HEAD SECTION - WORKING LINING HEAD SECTION - BACK UP LINING HEAD SECTION - INSULATION CHOKE SECTION - WORKING LINING CHOKE SECTION - BACK UP LINING CHOKE SECTION - INSULATION COOLER BREACHING SECTION - WORKING LINING BREACHING SECTION - INSULATION CUMILOX 101 HB (99.5% ALUMINA DENSE SHAPE) / CUMILOX 95 AZ SPL CUMICRETE CA 66 (94% ALUMINA DENSE CASTABLE) CUMICRETE CA 58 (94% ALUMINA INS. CASTABLE) CUMILOX 101 HB(99.5% ALUMINA DENSE SHAPE) CUMICRETE CA 66(94% ALUMINA DENSE CASTABLE) CUMICRETE CA 58(94% ALUMINA INS. CASTABLE) CUMILOX 101 HB(99.5% ALUMINA DENSE SHAPE) CUMIHICAST EXTRA (80% ALUMINA LCC) CUMICRETE C9 G (30% ALUMINA VERMICULTE BASED INS. CASTABLE)

23 Refractory Application in Hard Black Reactor Recommendation from CUMI APPLICATION AREA REFRACTORY HARD BLACK HIGH TEMPERATURE REACTOR TEMPERATURE ( Deg.C) HEAD SECTION - WORKING LINING HEAD SECTION - BACK UP LINING HEAD SECTION - INSULATION CHOKE SECTION - WORKING LINING CHOKE SECTION - BACK UP LINING CHOKE SECTION - INSULATION COOLER BREACHING SECTION - WORKING LINING BREACHING SECTION - INSULATION Spinel Zirconia Composite CUMICRETE CA 66 (94% ALUMINA DENSE CASTABLE) CUMICRETE CA 58 (94% ALUMINA INS. CASTABLE) CUMILOX 101 HB(99.5% ALUMINA DENSE SHAPE) CUMICRETE CA 66(94% ALUMINA DENSE CASTABLE) CUMICRETE CA 58(94% ALUMINA INS. CASTABLE) CUMILOX 101 HB(99.5% ALUMINA DENSE SHAPE) CUMIHICAST EXTRA (80% ALUMINA LCC) CUMICRETE C9 G (30% ALUMINA VERMICULTE BASED INS. CASTABLE)

24 APPLICATION AREA REFRACTORY HARD BLACK CONVENTIONAL REACTOR TEMPERATURE 1650 o C o C WORKING LINING QUENCH SECTION BREACHING SECTION - WORKING LINING BREACHING SECTION - BACK UP CUMILOX 101 HB (99.5% ALUMINA DENSE SHAPE, CUMILOX 201HF / CUMILITE 90 (90% ALUMINA DENSE SHAPE) CUMILOX 201 HF(90% ALUMINA DENSE SHAPE) CUMIHICAST 70 (70% ALUMINA LCC) HARD BLACK CONVENTIONAL REACTOR TEMPERATURE 1600 o C WORKING LINING BACK UP LINING & END PORTION HARD BLACK CONVENTIONAL REACTOR TEMPERATURE 1550 o C WORKING LINING INSULATION BACK UP Refractory Application in Hard Black Reactor Recommendation from CUMI CUMIHICAST SUPER(45% ALUMINA LCC) CUMILOX 201HF / CUMILITE 90, (90% ALUMINA DENSE SHAPE), CUMILITE WHF (FUSED MULLITE BASED 76% ALUMINA) CUMICRETE CK 588 (60% ALUMINA HIGH PURITY DENSE CASTABLE), CUMICRETE CK14 (50% ALUMINA HIGH PURITY DENSE CASTABLE) CUMILITE HF / WHF (FUSED MULLITE BASED 90 & 76% ALUMINA) CUMICRETE CK14 (50% ALUMINA HIGH PURITY DENSE CASTABLE)

25 Refractory Application in Soft Black Reactor (Typical Diagram of Carcass Reactor)

26 Refractory Application in Soft Black Reactor Recommendation from CUMI REACTOR TYPE APPLICATION AREA REFRACTORY LINING SOFT BLACK REACTOR TEMPERATURE o C SOFT BLACK REACTOR TEMPERATURE o C WORKING LINING BACK UP LINING & END PORTION WORKING LINING BACK UP LINING & END PORTION CUMILOX 95 AZ / CUMILOX 101 HB (99.5% ALUMINA DENSE SHAPE / BRICK) CUMILITE WHF (FUSED MULLITE BASED BRICKS / SHAPES) & CUMILAG B101 (98% ALUMINA INS. BRICK / SHAPES) CUMILITE HF / WHF ( FUSED ALUMINA BASED 90% AND 76% ALUMINA SHAPES) CUMICRETE CK 14 (50% ALUMINA HIGH PURITY DENSE CASTABLE)

27 Alumina Zirconia Composite : Choke Assembly for Hard Black Reactor Spinel Zirconia composite / Zirconia

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29 Refractory Application in Rotary Drier (Typical Diagram)

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31 Installation Service

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