Laboratory scaling of gypsum board production

The laboratory scale-up process of the production of gypsum boards is the fundamental basis for an efficient formulation development and thus, for the efficient production of high-quality gypsum boards.

1 Introduction

Gypsum based binders are widely used in construction. Combined with water and air, there are a huge variety of cost-competitive products which can be poured, sprayed or extruded to follow the desired forms for field or plant production. The apparent simplicity of gypsum chemistry is faced with complex technical production processes which are influenced i.e. by fluctuating gypsum raw material qualities and different calcining methods. Additionally, the complexity of the crystal structure formed depends on the hydration process as well as external parameters such as temperature and...

1 Introduction

Gypsum based binders are widely used in construction. Combined with water and air, there are a huge variety of cost-competitive products which can be poured, sprayed or extruded to follow the desired forms for field or plant production. The apparent simplicity of gypsum chemistry is faced with complex technical production processes which are influenced i.e. by fluctuating gypsum raw material qualities and different calcining methods. Additionally, the complexity of the crystal structure formed depends on the hydration process as well as external parameters such as temperature and the mixing process. Relevant physical and chemical pro­cesses can be controlled with admixtures. The ones commonly used are retarders, accelerators and plasticizers which often have to be tailored for specific binders and other varying application conditions. The challenge for gypsum producers is to find a formulation which allows cost-efficient production of high-quality gypsum products. The nature and concentration of the raw materials as well as their interactions control two critical parameters: workability and strength evolution [13]. Extensive efforts are generally made in the laboratory scale to find a correct combination of all components leading to the optimization and the control of the flow and setting properties. However, the materials prepared in the laboratory and in production can differ as their physical properties are also process dependent. The understanding of specific parameters such as the hydration kinetics, the rheology and mechanical properties of the gypsum slurry is crucial to successfully perform the scale-up from the laboratory to the production.

This paper describes a method to link production and laboratory by a continuous characterization of the physical properties during the process of gypsum board production, beginning with a review of the industrial process utilizing a generally common composition of the gypsum board. Due to the fast kinetics of the physical and chemical processes, different measuring tools had to be developed to study the rheological and mechanical properties of gypsum slurries. Conventional methods for mixing, testing of flow and setting time are then considered and compared with continuous characterization tools. Finally, the influence of selected process parameters like mixing intensity and additive formulation are presented.

2 Gypsum board production

Gypsum board production is a highly optimized continuous process involving the combination of three phases: (i) solid, (ii) liquid and (iii) gaseous which are evolving along the entire process. A general understanding of both – production process specialties and complex material composition – is mandatory to make possible the transition from the production to the laboratory.
2.1 A rapid continuous process
The production of gypsum boards is a continuous pro­cess which involves the mixing of powdered components, pre-generated foam and water containing different admixtures. The resulting slurry rapidly flows in less than 10 s on a cardboard layer with or without the help of vibration. The formed layer is later embedded with a second layer of cardboard. Typically, within less than 10 minutes, the plaster sets before the boards are cut to the desired length which occurs at the end of the production line. This first process step is shown schematically in Figure 1. A second step involves the drying of the board to remove excess water which is not required for the hydration process.

A complex formulation of foam, water, gypsum, but also additives like setting accelerator and plasticizer, is necessary to allow the efficient production of gypsum boards with its technical challenges. One of those challenges is the requirement for adequate fluidity in the initial seconds of processing, followed by rapid hardening and final gypsum board properties such as strength, density and cardboard adhesion.

2.2 Three phase system: water-powder-gas
The gypsum board formulation can be seen as the mix of three phases:
(i) liquid, containing water and admixtures like fluidizer,
(ii) solid with plaster powder (mainly b-CaSO4 ∙ ½ H2O) and solid additives, such as fine-ground gypsum (CaSO4 ∙ 2 H2O) as accelerator, and
(iii) gas i.e. air introduced with pre-generated foam.

 

A schematic representation of the gypsum board composition is made with the phase diagram shown in Figure 2. Generally, a mix of a solid powder and a liquid can lead to a suspension or slurry but also to a porous wet material. A liquid mixed with a gas leads either to a bubbly liquid or a foam. A solid-gas mix can be either a powder, granular or a dry porous material. Between the mixing and drying processes, plaster slurry is a mix of solid (mainly plaster powder), liquid (mainly water) and gas (pre-generated foam). During plaster hydration, a part of the water is consumed to form a wet porous material. The remaining excess water is evaporated in the drying phase, leading to the formation of the desired dry and porous gypsum board. The final gypsum board porosity largely determines the board density. This porosity is partially introduced with the foam but is also created during the drying process.

As is generally known, a greater amount of water is required to be added to form a flowable plaster slurry in comparison to the amount needed for the hydration. This has a negative impact on the final product strength. Additionally, higher drying efforts make a crucial contribution to the gypsum board production costs.

In order to reduce the quantity of excess water, plasticizer is commonly added to generate a certain workability or fluidity of the plaster slurry at lower water content [3]. Various plasticizer technologies exist which all have a different impact on the fluidity, the microstructure development and on the final strength. ­Special admixtures have been developed for gypsum-based applications [9, 11].

A minimum water content is needed (i) to control the fluidity of the pre-generated foam, (ii) for the chemical reaction, (iii) for the construction of the crystal network and (iv) for the adhesion to the cardboard. The amount of water needed for the fluidity can be reduced with the use of plasticizer or with the modification of the binder. However, to reach the desired board density the reduction of excess water must be compensated by the increase of the foam volume. An example of the effect of water reduction on the increase of foam volume is shown in Table 1. For three different water-binder ratios (W/G), different volumes and masses of main plaster slurry components are listed to produce a gypsum board of a desired final density of 0.8 g/cm3. The chemical expansion is not taken into account.

The reduction of the W/G from 0.8 to 0.6 leads to a 25 % reduction of the water added but also to a foam volume increase of more than 60 %. In addition to these basic physical considerations, the formulation has to be adapted taking the raw material specifications as well as various production process parameters into account. A quantitative characterization of the relevant physical properties is needed to link laboratory and production.

3 From the production to the laboratory: Scaling down

Scaling between production and laboratory is a major challenge in the industry, especially during the transition from product development to production. In the case of gypsum board production, this scaling is complex as it involves not only a scaling of the dimension and time, but also of the chemistry and the physics. The mixing of the powder with foam and water but also the setting and drying properties have to be characterized in both scales to enable the comparison. Therefore, quantitative measurements which can be performed in the laboratory as well as at the production line are needed. In this regard, the described high speed of gypsum board production is a special challenge. In the following, commonly used characterization methods are quantitatively compared with modern testing methods tailored for this application.
3.1 Material and methods:
quantification of mechanical properties
Relevant physical properties are commonly tested with a series of rapid test methods. Typical examples are presented in Figure 3: (i) slump flow test [10], (ii) knife-cut test for initial setting and (iii) thumb penetration for end of setting [5, 1]. Experience has shown that these relatively simple tests are directly linked with production, as Figure 3 schematically shows. A comparison between the laboratory measurements and the production justifies these tests, demonstrating their links but also their limitations. First of all, the mix of the three phases – liquid, solid and gas – is made in the production with a continuous mixer in typically less than 5 s, while it is i.e. mixed with a hand mixer in the laboratory in not less than 30 s. The mixture is then poured on to a cardboard layer, where the slurry has to be spread on the entire surface in a few seconds. In comparison, the slurry flow is tested and quantified in the laboratory with the slump flow at about 1 min after water addition. After less than 10 s, the slurry gets covered by a second layer of cardboard and after a few meters on the setting line (which corresponds to less than 1 min after water addition), the edges of gypsum boards are formed. At that point, the plaster slurry should no longer flow under its own weight. This limit is tested with the knife cut test where the poured slurry is cut with a knife to see if the slurry is no longer flowing and that it keeps its shape. In contrast, in the laboratory, this test is conducted not earlier than 1 min after water addition. At the end of the conveyor belt, after about 4 mins, the continuous layer of gypsum board is cut into the desired board lengths. The gypsum board should then bear the pressure imposed during the cutting step. The corresponding test in the laboratory – the so-called thumb pressure method – provides a result typically 5 to 10 min after water addition.

The laboratory tests mentioned principally correlate to the reality of the production except for two limitations: first the precision, as they are performed manually and secondly the kinetics, as it is much slower as compared to the actual production environment. As the rapid production of the gypsum board cannot be easily reproduced in the laboratory, both the formulation and the manufacturing process need to be adapted. Even if the classical tests emulate production, mostly no formulation can be found, which could be directly used in the production.

Alternative test methods exist which allow a continuous and precise characterization of the physical properties of binder slurries. Relatively simple to apply are the semi-adiabatic measurement of the temperature evolution [2] and conductivity [4]. However, these tests are not directly linked to the required physical properties of plaster slurries during setting and hardening. They can be measured i.e. with the Vicat test, ultrasonic measurements [8, 14] but also with classical rheological testing instruments like the rheometer [12, 14].

In the following, rheological measurements with an Anton Paar Physica MCR 301 rheometer are described. Due to the fast kinetics of the plaster hydration, a special geometry has been developed to measure the ­evolution of the shear modulus as a function of time. This geometry allows mixing of the powder with the water so that the evolution of setting and hardening can be analysed immediately after mixing. The powder is poured into the vessel containing the water and additives and mixed for 45 s at a constant shear rate of 500 s‑1. Then the temporal evolution of the stress is recorded with the same cell but in the flow mode, applying a shear rate of 0.01 s-1. At a stress of 200 Pa, the measurement is stopped to prevent damage to the measuring cell as a result of setting of the gypsum binder. To perform higher stress measurements, the use of plate/plate geometry with 10 mm diameter is chosen. A second measurement was performed with the same sample of the plaster slurry which is poured between two plates. The evolution of the complex modulus is recorded while a small shear deformation of 0.005 % is imposed. This plate/plate geometry can be used to measure a shear modulus of up to 2 ∙ 10Pa. The temporal shear modulus evolution of a plaster slurry (W/G = 0.7) prepared at different plasticizer concentrations versus corresponding slump flow, knife cut and thumb penetration ranges is represented in Figure 4. The figure shows results from an Anton Paar 301 rheometer with two different geometries (vane and plate-plate), a tailored ultrasound instrument and the classical tests. A good correlation between the classical tests and the continuous rheological characterization is found [14].

These measurements demonstrated in an exemplary way the correlation between ‘real’ physical values and classical testing methods. A complete quantitative comparison has already been described in a former paper [14].

A non-commercial instrument based on ultrasonic technology was developed at Sika Technology [2]. The testing device is schematically represented in Figure 5. It has also been used to follow the evolution of the shear modulus. Measurements made with the ultrasonic instrument and with the rheometer are comparable as can be seen in Figure 4. The ultrasonic technique leads to the same results as obtained with a rheometer but has the advantage of being transportable and easy to use.

As the testing device developed is mobile, it can be used either in the laboratory or at the production site. This allows a direct comparison of the results and a better comprehension of the link between the chemical evolution and the physical properties.

3.2 Selected parameters in production and laboratory
3.2.1 Setting of plaster slurry
The comparison of the setting of plaster slurry during production as well as in the laboratory has been made with both temperature and ultrasonic measurements. The temporal evolution of both measurements is represented in Figure 6. It demonstrates a large difference in the kinetics between the two scales, representing the described difference between laboratory and industry conditions. Even if no direct relationship can be established between the evolution of the shear modulus and the temperature, a temporal correlation between the initial chemical reaction observed with the temperature measurements and the strength evolution recorded with the ultrasonic measures can be found.

The temperature difference measured in the laboratory is lower than the one recorded in production as the thermal loss over a longer time scale is higher. Further factors must be taken into account to explain the differences observed between production and the laboratory. Those are, on the one hand, mix-design based whereby the final production mix differs from the laboratory-mix by (i) higher accelerator concentration and (ii) additional components like pre-generated foam and starch. On the other hand, process-related differences exist such as different mixing that occurs in a continuous mixer vs. a laboratory batch mixer. The effects of the mixing process and accelerator concentration are described below.

3.2.2 Effect of mixing on hydration
The mixing process is known to have a significant effect on the gypsum binder hydration [6]. In order to quantify this effect, a series of mixes are made with a Heidolph mixer where the motor speed is controlled from 100 to 2000 rpm for 30 s. The temperature evolution of the samples is then immediately recorded. Based on preliminary tests, the time needed to reach a temperature increase of 15 K correlates with the setting time [14]. The setting time as a function of the mixer speed is represented in Figure 7. A linear decrease of the setting time with the mixer speed is observed until a plateau is reached for the speed higher than 1000 rpm. Mixing energy has a significant impact on the plaster hydration kinetics: the phenomenon is classically explained with the mechanical destruction of the formed needle-shaped calcium sulfate dihydrate crystals under shear stress. This destruction involves an increase of the surface and of the number of nucleation centers, which are known to act as strong accelerators for the hydration of calcium sulfate hemihydrate. This has been confirmed by measuring the size distribution of particles after exposure to different mixing intensities [7, 12].

Tests performed in the laboratory are classically carried out with a Hobart mixer or even manually by hand stirring. In the latter case the mixing intensity varies significantly depending on the processor and can therefore lead to strong variations in the obtained setting time. The Hobart mixer gives more representative results but with 500 rpm the mixing speed is considerably different from the mixing intensity of a continuous mixer in a manufacturing environment. The hydration kinetics in the laboratory mix can therefore be linked to production by increasing the mixing intensity. This can be achieved either by increasing the mixing speed or the efficiency of the mixer. The mixing time, however, should be limited to minimize destruction of the newly formed structure. Even taking these aspects into consideration, the result of batch mixing in the laboratory will vary from continuous mixing during gypsum board production.

3.2.3 Accelerator concentration effect
Another important parameter during gypsum board production is the concentration of the accelerator which allows control of the hydration kinetics. The effect of the concentration of a classical accelerator based on fine ground gypsum is represented in Figure 8. As seen from laboratory tests, the setting time is decreasing logarithmically with the accelerator concentration. Assuming all other parameters are constant, this allows a precise prediction of the setting time with the concentration of the accelerator. The concentration of accelerator used in production is here around 0.2 % w/w and leads to a shorter setting time than found in the laboratory tests. The main reason for this difference is the mixing intensity which is lower in the laboratory preparation than in the production as has been discussed previously. Furthermore, a small quantity of hydrated calcium sulfate is permanently present in the continuous mixer which increases the real concentration of accelerator and thus accelerates the hydration.

4 Conclusions

Gypsum board production is highly dependent on many process parameters which can only be partially simulated in the laboratory. Currently, conventional test methods are severely limited in their precision and reproducibility. To overcome some of these limitations, Sika has developed a mobile method based on ultrasonic and temperature measurements. The evolution of the setting and hardening of plaster slurries has been evaluated and compared with traditional test methods. As an initial step, a quantitative comparison has been made with classical techniques in the laboratory and under real production conditions. The continuous evolution of setting and hardening of plaster slurry over time has not only been measured in the laboratory, but also directly during gypsum board production with high reproducibility. The influence of the mixing process and the effect of additives have been shown by way of an example.

This investigation confirms that the development of a gypsum board formulation is not an easy task; however, it can be simplified by using modern testing methods. The flow and setting properties are closely dependent on the nature of the gypsum raw material and the calcination process. Admixtures are required to regulate the gypsum board production process. For the sometimes widely varying requirements specifically tailored additives need to be developed. A targeting formulation is obtained with a series of lab-tests which mimic the production process as closely as possible. The easy-to-use methods presented allow continuous quantitative characterization of the major chemical and physical material properties. In addition, using these mobile devices, it is possible to reduce the time and effort to scale up from the laboratory to the production by reducing the number of plant trials resulting in significant cost savings.

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