APPARATUS AND METHOD FOR PRODUCING AND ANALYZING A PLURALITY OF SAMPLE MATERIALS

Abstract

An apparatus for producing and analyzing sample materials may comprise a milling device for milling material components, a first metering device for metering a material component into the milling device, a second metering device for metering an activator liquid into the milled material component, a homogenization device for homogenizing the material components and the activator liquid to produce a sample material, a control device that is connected to the milling device and is configured to vary a parameter characteristic for milling intensity of the milling device so that particle size of the material components is altered, and a measuring device for determining a reactivity of the sample material. The present disclosure further concerns a process for producing and analyzing a plurality of sample materials. The process may involve varying at least one parameter characteristic for milling intensity for each sample material produced.

Claims

1.-15. (canceled)

16. An apparatus for producing and analyzing sample materials, the apparatus comprising: a milling device for milling material components; a first metering device for metering at least one of the material components into the milling device; a second metering device for metering an activator liquid into the at least one of the material components that has been milled in the milling device; a homogenization device for homogenizing the material components and the activator liquid to produce a sample material; a control device that is connected to the milling device and is configured to vary a parameter characteristic for a milling intensity of the milling device so as to alter particle size of the material components; and a measuring device for determining a reactivity of the sample material.

17. The apparatus of claim 16 wherein the measuring device is a colorimetric measuring device.

18. The apparatus of claim 16 wherein the control device is connected to the first metering device and is configured to control a metered amount of the at least one of the material components.

19. The apparatus of claim 16 wherein the first metering device is heatable.

20. The apparatus of claim 16 further comprising a crushing device disposed upstream of the milling device.

21. The apparatus of claim 16 further comprising a rheometric measuring device for determining rheological properties of the sample material.

22. The apparatus of claim 16 further comprising a sample store with a plurality of sample containers for accommodating sample materials.

23. The apparatus of claim 16 wherein the measuring device is configured to simultaneously determine reactivities of a plurality of sample materials.

24. The apparatus of claim 16 further comprising a third metering device for metering a cement additive into the at least one of the material components downstream of the milling device.

25. A process for producing and analyzing a plurality of sample materials, the process comprising: metering a material component into a milling device; milling the material component in the milling device; metering an activator liquid into the material component; homogenizing the material component and the activator liquid to produce a sample material; repeating the above steps to produce a plurality of sample materials, wherein a parameter characteristic for a milling intensity is varied for each of the plurality of sample materials produced; and determining a reactivity of each of the plurality of sample materials with a calorimetric measuring device.

26. The process of claim 25 wherein at least one of a speed of rotation of the milling device or a milling time of the material component is varied during the milling of the material component in the milling device.

27. The process of claim 25 further comprising determining rheological properties of the plurality of sample materials.

28. The process of claim 25 further comprising crushing the material component prior to milling the material component in the milling device.

29. The process of claim 25 wherein the metering of the material component into the milling device comprises heating the material component.

30. The process of claim 25 further comprising determining particle size of at least part of the milled material component prior to homogenizing the material component.

Description

PREFERRED WORKING EXAMPLES OF THE INVENTION

[0034] The invention is illustrated below by means of a number of working examples with reference to the accompanying figures.

[0035] FIG. 1 schematically shows an apparatus for analyzing a sample material as per one working example.

[0036] FIG. 2 schematically shows an apparatus for analyzing a sample material as per a further working example.

[0037] FIG. 1 schematically shows an apparatus 10 for analyzing a sample material. The analysis apparatus 10 has, by way of example, three containers 12, 14 and 16 in each of which a material component is stored. The depiction of three containers 12, 14, 16 is merely by way of example; it is conceivable to provide many containers each containing a material component in the analysis apparatus 10.

[0038] The material components are in particular material components of a binder such as cement. For example, clinker such as portland cement clinker or sulfoaluminate clinker together with a sulfate carrier and additives are used for producing binders. A sulfate carrier is, for example, gypsum, hemihydrate, anhydrite or other materials having an elevated SO.sub.3 content. Additives are, for example, latently hydraulic materials, slag sand, brown coal fly ash, silica dust or pozzolans such as hard coal fly ash, natural pozzolans, synthetic pozzolans or filler materials such as limestone. The material components are stored in the containers 12, 14, 16, preferably as crushed material having a particle size of up to 3 mm, as powder having a particle size of up to about 0.09 mm or as granules having a particle size of from about 3 to 10 mm.

[0039] The analysis apparatus 10 additionally has a first metering device 18 which is connected to the containers 12, 14 and 16. The metering device 18 is, for example, a weighing cell, a balance or a volumetric measuring device. The metering device conveys a particular amount of the material components out of the respective container 12, 14, 16. The metering accuracy of the metering device is, based on the total amount weighed out, about 0.01-1%, preferably 0.007%-0.25%, most highly preferably about 0.5%.

[0040] A milling device 20 is installed downstream of the metering device 18. The milling device 20 is, for example, an oscillatory disk mill or a vibratory mill. The metering device 18 meters a particular amount of a material component from one of the containers 12, 14 and 16 into the milling device 20. The material components are, for example, conveyed directly from one of the containers 12, 14, 16 via the metering device 18 to the milling device 20 or combined in an intermediate store (not shown) and subsequently fed together to the milling device 20.

[0041] The milling device 20 is followed by a further optional metering apparatus 22 and a homogenization device 24, a second metering device 26 for metering an activator liquid and a sample store 30 having a plurality of sample containers 28.

[0042] The analysis apparatus 10 additionally has a calorimetric measuring device 32 for determining the reactivity of a sample material and also a rheometric measuring device 34 for determining the processing properties of the sample material.

[0043] Furthermore, the analysis apparatus 10 has a control device 38 which is connected to the first metering device 18, the milling device 20, the activator liquid metering device 26, the homogenization device 24 and the measuring devices 32 and 34.

[0044] In an analysis method by means of the analysis device 10, a particular composition of the sample material can be set via the control device 38. The proportions of the material components from the containers 12, 14, 16 in the sample material can, for example, be set manually on the control device 38 or can be calculated by the control device 38 at a predetermined interval, so that a plurality of sample materials having a proportion of a material component which varies over a particular quantity interval can be analyzed. The control device 38 is connected to the metering device 18 in such a way that the metered amount of material components set on the control device 38 is metered by means of the metering device 18 from the containers 12, 14, 16 into the milling device. The material components are subsequently milled individually or together in the milling device 20. In the case of joint milling of the material components, the material components are metered in succession into a sample container which is not shown in FIG. 1 and subsequently fed to the milling device.

[0045] The speed of rotation or the speed of vibration of the milling device 20 and also the duration of the milling process and thus the milling intensity can, for example, be set via the control device 38. A particular fineness of the sample material can thus be set on the milling device 20 via the control device 38.

[0046] After the milling device 20, the sample material is metered by means of a metering apparatus 22 into a sample container 28. The metering apparatus 22 determines, for example, the net weight of the sample material introduced into the sample container 28. For example, the metering device determines the net weight of the sample container 28, the total weight of the sample container 28 with the sample material and/or the net weight of the sample material introduced into the sample container 28.

[0047] The sample container is arranged in a sample store 30 which has a plurality of sample containers 28 which, for example, each contain different sample materials. In the working example depicted in FIG. 1, the sample store encompasses sixteen sample containers 28 which are arranged in four rows.

[0048] The above-described steps are preferably repeated with variation of the parameters which can be controlled by the control device 38, so that a plurality of different sample compositions are arranged in different sample containers 28 in the sample store 30.

[0049] An activator liquid is fed via the activator liquid metering device 26 into the sample container 28. If one of the material components is portland cement clinker or sulfoaluminate clinker, water is metered as activator liquid into the sample container 28. If one of the material components is a geopolymer, an alkali solution is metered as activator liquid into the sample container 28. The activator liquid metering device 26 has, for example, a heating device for heating the activator liquid, in particular to the temperature of the calorimetric measuring device 32. The metering accuracy of the metering device 26 is not more than about 0.001-1%, preferably 0.007-0.25%, most highly preferably about 0.5%, of the desired metered amount.

[0050] In particular, an activator liquid is metered via the activator liquid metering device 26 into the material components in the sample container 28 so that the ratio of liquid to sample material is about 0.25-1.2, in particular 0.4-0.6, particularly preferably 0.45-0.55. The activator liquid and the material components are homogenized in the sample container in the homogenization device 24 to give a sample material. The homogenization device 24 comprises, for example, a vibratory apparatus by means of which the sample container is subjected to vibration. The homogenization 24 can also be carried out by means of mechanical mixing such as stirring or knocking.

[0051] The sample container 28 in the sample store 30 is subsequently introduced into the calorimetric measuring device 32. It is likewise conceivable to introduce the sample container separately, without sample store 30, into the calorimetric measuring device 32.

[0052] The addition of the activator liquid to the material components starts the hydration process, with the energy stored in the material components being liberated in the form of heat of reaction. The sample container 28 is therefore introduced into the measuring device 32 immediately after addition of the activator liquid and the subsequent homogenization, so that the entire heat of reaction liberated is preferably measurable. For example, the heat of reaction is energy in the clinker stored beforehand in the mineral phases by cooling in a clinker cooler. This heat of reaction is characteristic of the reactivity of the mixture of the material components. The cumulative energy liberated to any point of time during hydration corresponds to the weighted average of the contribution of the individual material components. The degree of hydration and the hydration rate is determined by the mineralogical composition of the material components, in particular the clinker, the sulfate carrier added and the surface area produced during milling of the material components. The hydration reaction proceeds isochemically, with the freshly formed hydrate phases being largely X-ray amorphous.

[0053] The calorimetric measuring device 32 is configured in such a way that it determines the heat given off by the sample material over a particular period of time.

[0054] Commercially available calorimeters, for example isothermal heat flow calorimeters, make it possible to determine the heat of hydration of a plurality of different sample materials in parallel over a particular time. Known calorimeters have a plurality of measuring channels in which different sample materials are analyzed at the same time. The calorimetric measuring device 32 is configured in such a way that small sample quantities, for example 1-10 g, preferably 3-8 g, very highly preferably about 5 g, are sufficient for determining the reactivity of the sample material. The measuring device 32 determines the heat of hydration over, for example, a measurement time of about 1-8 days, in particular 4-6 days, preferably 5 days, at a temperature in the calorimeter of about 20-45° C., in particular 20-27° C. Raising the temperature to about 45° C. makes a short measurement time of less than one day also conceivable.

[0055] The calorimetric measuring device 32 transmits the measurement result to the control device 38. The control device 38 is, furthermore, configured in such a way that it determines a reactivity of the sample material by means of the heat given off by the sample material, as determined by the calorimetric measuring device.

[0056] Between the elements of the analysis apparatus 10, there are, for example, transport devices such as conveyor belts, mobile robots or fixed-position robots having a long reach which are shown schematically as arrows in FIGS. 1 and 2.

[0057] FIG. 2 schematically shows an apparatus 11 for analyzing a sample material as per a further working example. The analysis apparatus 11 has all elements of the analysis apparatus 10 described with reference to FIG. 1, with the metering device 18 of the analysis device 10 having been replaced by three metering devices 40, 42, 44 and the metering device 40 additionally having a heating device 46. Furthermore, the analysis device 11 of FIG. 2 has a further crushing device 36 located upstream of the milling device 20 and also a third further metering device 48 for metering solid or liquid additives, for example milling aids (e.g. DEG, TEA) or cement additives (e.g. TIPA, CaCl.sub.2) into the sample container 28.

[0058] The analysis apparatus 11 also has a rheometric measuring device 34 for determining the rheological properties of the sample materials in the sample containers 28 of the sample store 30.

[0059] The analytical method which can be carried out by means of the analysis apparatus 11 corresponds substantially to the analytical method described with reference to FIG. 1, with each of the containers 12, 14, 16 being assigned a metering device 40, 42, 44 which meters an amount of material components which can be set by means of the control device 38 into the crushing device 36. The metering device 40 which is assigned to the container 16 has a heating device 46 by means of which the material component from the container 16 is heatable. The material component in the container 16 is, for example, a sulfate carrier which is heated and thus thermally dewatered by means of the heating device 46.

[0060] The crushing device 36 breaks, in particular, material components having a large particle size, e.g. granules having a particle size of from about 3 to 10 mm, before introduction of the material components into the milling device 20.

[0061] Furthermore, the analytical method by means of the analysis apparatus 11 comprises a rheometric measurement by means of the rheometric measuring device 34. The rheometric measuring device 34 determines the rheological properties, for example the flow limit, of at least part of the sample material in the sample containers 28 of the sample store 30.

[0062] In the analysis apparatuses 10 and 11, parameters such as the proportions by mass of the material components from the containers 12, 14, 16 in the sample material, the degree of milling of the material components and the amount of activator liquid and additives of the sample material can be set by means of the control device, so that it is possible to produce many sample materials for which one or more parameters vary in a known manner. Analysis of the plurality of sample materials in a sample store 30 at the same time in the calorimetric measuring device 32 makes it possible to determine the reactivity of a material as a function of particular parameters such as particle size and composition of the material in a simple manner. Furthermore, the analysis device 10, 11 makes it possible to produce a large number of sample materials in a simple manner and thus produce a high data density based on the variation of the parameters. This makes precise analysis, in particular of nonlinear relationships between the reactivity or the rheological properties and the parameters of the sample materials, e.g. composition and particle size, possible.

LIST OF REFERENCE NUMERALS

[0063] 10 Analysis apparatus [0064] 11 Analysis apparatus [0065] 12 Store [0066] 14 Store [0067] 16 Store [0068] 18 First metering device [0069] 20 Milling device [0070] 22 Metering device [0071] 24 Homogenization device [0072] 26 Second metering device for metering an activator liquid [0073] 28 Sample container [0074] 30 Sample store [0075] 32 Measuring device [0076] 34 Measuring device [0077] 36 Crushing device [0078] 38 Control device [0079] 40 Metering device [0080] 42 Metering device [0081] 44 Metering device [0082] 46 Heating device [0083] 48 Third metering device