A Study on the Flame-Retardant Performance of Recycled Paper Building Materials Manufactured by 3D Printer

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Reviewer Comments

Reference

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Reference

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1

Please include who did the research and the objective of this research.

Amat, R.C.; Ibrahim, N.M.; Rahim, N.L.; Tajudin, N.S.B.A.; Ahmad, K.R. Fire Resistance of Biomass Ash Panels Used for Internal Partitions in Buildings. Procedia Engineering 2013, 53, 52–57

Amat et al., the study was conducted to develop a refractory partition based on the oil extraction process's waste residual biomass EFP (Empty Fute Bunch). As a result of the study, the developed biomass material (EFB) panel board showed fire resistance at a compressive strength of 3.535 MPa for more than 2 hours.[11]

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Include the exact value of the flame retardant result. Superior is too general.

Rie, D.-H.; Moon, S.-W.; Lim, K.-B. Combustion and Thermal Properties of Paper Honeycomb: Treatment of Phosphorus-Based Flame Retardant Agents. J Therm Anal Calorim 2012, 107, 535–539

Rie et al., After the specimen was produced using a phosphorus flame retardant in the paper honeycomb structure, flame retardancy evaluation was conducted using a cone calorimeter. The flame-retardant performance evaluation using a cone calorimeter showed an 84.2 % improvement in the flame-retardant impregnated specimen compared to the untreated specimen.[12]

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Include following references

Mohd Basri, M.S.; Mustapha, F.; Mazlan, N.; Ishak, M.R. Rice Husk Ash-Based Geopolymer Binder: Compressive Strength, Optimize Composition, FTIR Spectroscopy, Microstructural, and Potential as Fire-Retardant Material. Polymers

Basri et al., conducted a study on the correlation between fire resistance and compressive strength of the synthetic material of the rice husk (RHA)-based geopolymer binder (GB). Factors selected in this study were rice husk ash/active alkali solution (RHA/AA) ratio and sodium hydroxide (NaOH) concentration. RHA-based GB has excellent fire resistance (slow, thermally stable combustion) and mechanical properties, making it highly likely to be used as an insulating material in various fields.[14]

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Zuo, B.; Yuan, B. Flame-Retardant Cellulose Nanofiber Aerogel Modified with Graphene Oxide and Sodium Montmorillonite and Its Fire-Alarm Application. Polymers for Advanced Technologies 2021, 32, 1877–1887

Zuo and Yuan manufactured aerogels to study the improvement of insulation and pressure resistance of insulation materials. In this study, graphene oxide (GO), montmorillonite (MMT), and cellulose nanofibers (CNF) were used to make an aerogel using a vacuum freeze-drying method. As a result, aerogels have the advantage of improving insulation performance and flame retardant performance by reducing the thermal conductivity of insulation materials.[15]

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Wang, Y.; Hou, M.; Zhang, Q.; Wu, X.; Zhao, H.; Xie, Q.; Chen, J. Organophosphorus Flame Retardants and Plasticizers in Building and Decoration Materials and Their Potential Burdens in Newly Decorated Houses in China. Environ. Sci. Technol. 2017, 51, 10991–10999

Wang et al., a study conducted to measure the Organophosphorus flame retardants (OPFRs) concentration of products using OPFRs for flame retardant performance. As a result, OPFRs concentrations differed significantly from 14.78 ng/g (putty powder) to 9649000 ng/g (expanded polystyrene panel (EPS). The expected burden of OPPR for interior decoration using nonwoven wallpaper was 330 times and 2110 times higher than when latex paint and diatomite were used, respectively. [18]

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Is the ceramic binder an additive? Please clarify

The ceramic binder used as the main additive was "FP-100" produced by Sunjin Chemical Co., Korea.

The ceramic binder of this study was the main additive, and 'FP-100' produced by Sunjin Chemical Korea was used.

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"..48% MgO, 17% SiO2, and 14.6% Al2O3." These components not account for 100%. What percentage of other components?

The ceramic binder components consisted of other components, including 48% MgO, 17% SiO2, and 14.6% Al2O3.

The ceramic binder components consisted of including 48% MgO, 17% SiO₂, 14.6% Al₂O₃, 12% Illite, 7% ZrO₂, 1% Al₂O₃, 0.8% Fe₂O₃, 0.6% CaO.

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Section 3.1, 3.2, 3.3, 4.1 must be under Method and Materials. Please rearrange

3. Making a Specimen and Physical Characteristics

3.1 Wet Cellulose 3D Printer

3.2 Cellulose Filament Production

3.3 WC (Wet Cellulose)-3D Printing

3.4 Specimen and Physical Characteristics

4.1. Description of ISO 11925-2 test

4.2 Results of ISO 11925-2 Test

2.1 Making a Specimen and Physical Characteristics

2.2 Wet Cellulose 3D Printer

2.3 Cellulose Filament Production

2.4 WC (Wet Cellulose)-3D Printing

2.5 Specimens and Physical Characteristics

2.6 Description of ISO 11925-2 test

3. Results of ISO 11925-2 Test

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Explain how the calibration was conducted for the self-developed WC-3D Printer before it was used.

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The WC-3D printer includes automatic zeroing. The zero position is marked in the center of the work surface and can be checked from the outside when the printer's automatic zero adjustment devices are operated. If it was necessary to change the position, we changed the position of the limit sensor on the X-axis and Z-axis and changed the position of the BL touch sensor on the Y-axis.

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Please explain in detail how the machine works. How many waste paper used, how many water etc.

Pulping of the waste paper was performed by separating the waste paper from water. The operating conditions of the pulping equipment were set to a capacity of 16L with a motor speed of 360 RPM and an operating time of 60 minutes. Figure 3 shows the pulp equipment and the resulting pulp

Pulping of the waste paper was performed by separating the waste paper from water. The operating conditions of the pulping equipment were set to a capacity of 16L with a motor speed of 360 RPM and an operating time of 60 min. Figure 3 shows the pulp equipment and the resulting pulp. Pulper dissociated the paper weight/water weight ratio (wt%) at a ratio of 1/2.5 to 3 times.

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PAM (PolyAcrylaMide) was used as well but not included in Table 2. It only mentioned within 5 wt%. Is it 5 or 4 or 3 wt%. Within is an ambiguous word.

PAM was added as a dispersion material of 3D printing extrusion and mixture material within 5 wt%.

PAM was added as a dispersion material in 3D printing extrusion and mixture material 5 wt%.

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Please give reasoning why ceramic binder of 10 wt% is not consider for the design in Table 2

Through its preliminary experiment, it was confirmed that the performance was implemented in the content ratio of the ceramic binder of 20 wt% or more, and a specimen of 10 wt% was not manufactured.

It has already been described in the text above in Table 2 of 2.3 Cellulose Filament Production.

The contents of the paper :

Through a preliminary experiment, it was confirmed that the performance was implemented in a content ratio of the ceramic binder of 20 wt% or more, and a specimen of 10 wt% was not manufactured.

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The mixing ratio of cellulose filaments is weight% (wt%) as a weight ratio of the number of additives based on the weight 100 of waste paper." Hard to understand. Please rephrase.

The mixing ratio of cellulose filaments is weight% (wt%) as a weight ratio of the number of additives based on the weight 100 of waste paper.

Cellulose filaments for 3D printing were based on 100 wt% waste paper. The additives were adjusted in a weight ratio to 100 wt% of the waste paper, and the unit was weight% (wt%).

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What is the reason in displaying sample before and after drying? Is it have any effect on your results? Please clarify.

Table 3 shows the appearance before and after drying the output specimen.

Table 3 shows the appearance before and after drying the output specimen. From the images in Table 3, it was confirmed that the specimen before drying contained a lot of moisture for 3D printing, but it did not bring shape deformation as the moisture evaporated during the drying process.

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Why the weight after dry for sample with 30 wt% is almost similar to the sample with 30 wt%? Silimarly with the sample with 40 and 50 wt%? Please include reasoning.

The average weight of a specimen before drying was 784g. Figure 3 shows the average weight of a specimen after drying. The average weight of a specimen after drying was 113g.

The average weight of a specimen before drying was 784g. Figure 3 shows the average weight of the specimen after drying. The average weight of a specimen after drying was 113g. The filling process of the cylinder filament was performed manually. In this process, it is assumed that a fine air layer was formed inside the cylinder. The amount of filament extrusion of the printer was associated with the number of rotations of the motor. Therefore, it is presumed that although the motor was appropriately rotated and extruded from the cylinder, fine air came out instead of the filament. It is assumed that a weight error occurred in this part, and the error range was confirmed to be ±1 g.

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Please label Figure 5 (a) and (b).

Figure 5. An ISO 11925-2 Experimental Device. (b) ISO 11925-2 Test

Figure 5. (a) An ISO 11925–2 Experimental Device. (b) A test prepared (c) ISO 11925–2 Test

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Please decribe the method of the testing in detail.

What is the angle of the flame?

What is the temperature of the flame

The ISO 11925-2 test method applied to this experiment was to investigate the characteristics of the vertical direction fire propagation of materials inside and outside the building. Therefore, the material was installed in a vertical direction and has the characteristic of being directly heated in a single frame regardless of the radiated heat. Therefore, in this experiment, it was possible to evaluate the fire protection performance by directly exposing the building material to a flame and measuring the carbonization area, and then comparing it.

In the ISO 11925-2 experiment, the extended flame (21 mm height) and execution time (30 seconds) was applied to understand the characteristics of flame retardant performance in detail. The sample was kept constant at a relative humidity of 23(±2)°C and 50(±5)% for 2 days and then continued

The purpose of the ISO 11925–2 test method applied to this experiment was to investigate the vertical fire propagation characteristics of materials inside and outside a building. The specimen was pretreated at 23(±2)°C and 50(±5)% relative humidity for two days using a constant temperature and humidity (constant humidity spec). The pretreated specimen was exposed to flames for 30 seconds using an ignition source inclined 45 degrees relative to the vertical axis. The ignition source used this time is prepared to have a height of 21mm by adjusting the gas supply valve in a vertical position using commercial propane (between 10KPa and 50KPa) with 95% purity. The specimen is positioned and fixed between two U-shaped frames made of stainless steel, represents 40 mm as a reference line on the bottom surface, and represents a reference line of 150 mm upward from the reference line. The experiment was terminated after 30 seconds when the timer was activated at 45 degrees and the flame met the specimen.

This experiment is installed vertically and has the property of heating directly in a single frame regardless of radiant heat. Therefore, in this experiment, the fire protection performance could be evaluated by directly exposing the building materials to flames and measuring and comparing the carbonized area.

At the end of the experiment, the performance standard was evaluated by applying the standard of EN 13501–1. [24]

Reference:

24. British Standards Institution Reaction to Fire Tests. Ignitability of Products Subjected to Direct Impingement of Flame. Part 2, Single-Flame Source Test.; 2020;

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"One of the eight specimens in which a deep fire..". Which specimens?

One of the eight specimens in which an after-glowing occurred evolved naturally and seven specimens were confirmed to be completely burned.

One of the eight specimens in which an after-glowing occurred evolved naturally and seven specimens were confirmed to be completely burned. It was confirmed that an after-glowing of 30 wt%-3 specimens was extinguished naturally over time.

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"As the amount of ceramic binder added increased, the average flame propagation height decreased.". Describe why.

As the amount of ceramic binder added increased, the average flame propagation height decreased

The average damage height according to the ceramic content of the sample was 0 wt% 176.7mm, 20 wt% 92.3mm, 30 wt% 63mm, 40 wt 56.7mm, and 50 wt% 49mm, which confirmed that the carbonization length decreased as the content of the ceramic binder increased.

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"The ISO 11925-2 test confirmed that a 40 wt% ceramic binder-added specimen ensures flame-retardant performance.". Why 40 and not 50 wt%?

The ISO 11925-2 test confirmed that a 40 wt% ceramic binder-added specimen ensures flame-retardant performance.

According to the ISO 11925–2 test, it was confirmed that the damage height, which is a performance standard of EN 13501–1, was measured within 150mm without after-glowing in a sample of 40 wt% of a ceramic binder, and thus the minimum content was ensured for flame retardancy.

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"..had no flame retardant performance as cracks and holes penetrating the specimens..". Describe why?

Also, it was determined that the specimens of 30wt% or less of the ceramic binder had no flame retardant performance as cracks and holes penetrating the specimens and after-glowing were identified.

Also, a sample of 30 wt% or less of the ceramic binder was judged to be unable to be used as a building material because of the same hole pattern of the after-glowing as the fire propagation characteristics of the general combustible material.

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"The specimens with an amount of 40wt% or more of the ceramic binder added had a damage height within 150 mm that satisfies the performance standard of EN 13501-1.". Specimens with 20 and 30 wt% ceramic binder also had damage height below 150mm. Please explain.

The specimens with an amount of 40wt% or more of the ceramic binder added had a damage height within 150 mm that satisfies the performance standard of EN 13501-1.

The damage height of the sample to which 20 wt% or more of a ceramic binder was added was within 150 mm. However, an after-glowing occurred in samples with ceramic binder contents of 20 wt% and 30 wt%, and the entire sample was burned. Therefore, in this study, a specimen containing 40% by weight of the ceramic binder prevented the vertical diffusion of fire and did not generate an after-glowing, so it was determined as the minimum content.

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Please include discussion with several references. The discussion is not supported by any references.

The specimens with an amount of 40wt% or more of the ceramic binder added had a damage height within 150 mm that satisfies the performance standard of EN 13501-1. And it was confirmed that after-glowing did not appear.

The damage height of the sample to which 20 wt% or more of a ceramic binder was added was within 150 mm. However, an after-glowing occurred in samples with ceramic binder contents of 20 wt% and 30 wt%, and the entire sample was burned. Therefore, in this study, a specimen containing 40% by weight of the ceramic binder prevented the vertical diffusion of fire and did not generate an after-glowing, so it was determined as the minimum content.

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1

Abstract: Please, at first describe the meaning of "WC" (Wet Cellulose) in the text.

This study developed its 3D printer cellulose filaments. In addition, a cellulose filament composite material was developed using additives wastepaper-based cellulose for printing. After manufacturing a specimen using a WC 3D printer, a reliability test for the flame-retardant performance of the material was conducted according to the ISO 11925-2 test method.

In this study, the self-developed WC (Wet Cellulose)-3D printer confirmed the standardization and uniform performance of the sample by filling the material supply cylinder with cellulose filaments and spraying the composite material through a 10 mm nozzle. The cellulose filament for a WC-3D printer is based on cellulose extracted from waste paper, and a cellulose filament composite material is used by mixing additives. After manufacturing a specimen using a WC 3D printer, a reliability test for the flame-retardant performance of the material was conducted according to the ISO 11925-2 test method.

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Conclusion part-please add the future direction of your research from a practical point of view.

Finally, it was confirmed that cellulose filaments containing 40 wt% or more of ceramic binders can produce building materials of various shapes capable of preventing fire diffusion using a WC 3D printer.

Finally, it was confirmed that cellulose filaments containing 40 wt% or more of ceramic binders can produce building materials of various shapes capable of preventing fire diffusion using a WC 3D printer.

Through this study, the possibility of developing building materials with flame-retardant performance using waste paper-based cellulose was confirmed. Additionally, further research on the flame retardancy performance of customized building materials using the WC-3D printer is needed.

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