CN109406343B - Method for obtaining rheological parameter range of wall putty construction - Google Patents
Method for obtaining rheological parameter range of wall putty construction Download PDFInfo
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Abstract
The invention discloses a method for acquiring rheological parameter range of wall putty construction, which comprises the following steps of S1, sampling according to the requirements of a rotational rheometer; s2, performing rheological test; s3, carrying out data processing on the shear stress-shear rate data points obtained in the step S2 to obtain rheological parameters of the putty sample; s4, obtaining rheological parameters of a plurality of putty samples according to the steps S1-S3, and selecting a rheological parameter range with the putty construction performance reaching the standard according to the construction performance of each putty sample. In the prior art, in the process of testing a putty sample, under the condition of high shear rate, data obtained by a testing device commonly used in the industry has the defects of serious fluctuation, low fitting index, poor repeatability and the like.
Description
Technical Field
The invention relates to the field of engineering materials, in particular to a method for acquiring a rheological parameter range of wall putty construction.
Background
Currently, wall putties are mainly constructed by experienced builders through batch scraping by means of batch knives and putty knives. When the putty powder and putty paste products for interior walls are developed or improved, the formula and process adjustment for optimizing the construction performance mainly depend on the simulation of site construction by experienced constructors, and then a plurality of construction performance indexes are graded item by item. And the formula design engineer adjusts the formula according to the grading result. In the construction performance scoring project, the batch scraping hand feeling is the most important factor for determining the grade. The grading result of batch scraping hand feeling of a constructor is greatly influenced by human subjective factors, and the grading results given by different people, even the same person at different time can be inconsistent. This uncertainty in scoring results due to inconsistent subjective human factors has greatly interfered with the development of product formulations. Meanwhile, in the aspect of controlling the quality stability of the delivered product, a set of objective and reliable technical indexes is urgently needed to measure the batch scraping hand feeling of the putty product.
The method for evaluating the construction performance of the putty product in the industry standard of the building industry is greatly different from the actual construction condition. The construction performance description of the putty for the inner wall of the JG/T298-2010 building and the putty for the outer wall of the JG/T157-2009 building has 'barrier' or 'barrier-free', the subjective component is large during judgment, and no digital parameter limit standard exists. The evaluation of the construction hand feeling of the putty product in the factory inspection still depends on the subjective scoring method of the real hand feeling of the skilled constructor in the putty batch scraping process at present. Although the method can quantify, the number for quantification comes from subjective feeling, the score is difficult to directly correlate with the composition of the formula, and therefore an objective quantitative index capable of correlating the formula, the process and the actual construction performance is needed, and the quantitative index corresponds to the actual construction performance. In evaluating the workability of the putty, the most important is the hand feel of the constructor during the batch scraping process. The quantitative research on putty batch scraping handfeel is mainly based on rheological characteristics of materials, and the workability of the materials is evaluated by taking inherent rheological parameters of the materials as indexes. The rheological parameters of the sample in the aspects of fluidity, plasticity and the like can be obtained by means of a rotational rheometer, a rotational viscometer, a puncture depth meter, a consistometer, a jump table and the like. For example, the method for evaluating the workability of putty in the domestic construction putty industry is a consistometer (GB/T1749), and the construction material industry in North America and Europe generally uses a diving-table (Belgian standard NBN B13-206) and an Emley Plasticity Meter (American ASTM C110-04.7) to measure the quality of the workability.
Both the consistometer and the diving table standard test methods examine the static yield stress of a material from rest to before flowing, which is not exactly the same as the rapid spreading process of actual putty or mortar during batch scraping. The putty is semi-solid and has strong thixotropy. Some samples have large thickness values measured by a consistometer, but have good batch scraping hand feeling, so that the use of the thickness value as a single evaluation index can cause misleading to formula adjustment. In addition, the measurement results of the two simple instruments are greatly influenced by operators, and the comparability between data obtained by different operators is poor.
Aiming at the structural characteristic of small surface layer putty filler, the invention obtains good repeatability and reproducibility data while objectively reflecting the batch scraping hand feeling of the putty by means of a high-precision rotational rheometer, and determines the rheological parameter range suitable for formula development and quality control according to a large amount of data.
The present invention has been made in view of this situation.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for acquiring the rheological parameter range of wall putty construction, which adopts a rotary rheometer to test and reasonably selects the range of each parameter in the test, thereby overcoming the defect of large error of experimental data.
In order to solve the technical problems, the invention adopts the technical scheme that the basic concept is as follows:
a method for acquiring a rheological parameter range of wall putty construction comprises the following steps:
s1, sampling the putty sample according to the sampling requirement of the rotational rheometer and loading the putty sample;
s2, rheology test: standing the putty sample for 2min, starting testing, collecting a plurality of torque and corresponding rotating speed signals, and respectively calculating and outputting shear stress-shear rate data points;
s3, carrying out data processing on the shear stress-shear rate data points obtained in the step S2 to obtain rheological parameters of the putty sample, wherein the rheological parameters comprise yield stress and plastic viscosity;
s4, obtaining rheological parameters of a plurality of putty samples according to the steps S1-S3, and selecting a rheological parameter range with the putty construction performance reaching the standard according to the construction performance of each putty sample.
Preferably, before step S1, the method further includes a process of pre-treating the putty sample: adding water into a putty sample (putty powder) according to a specified proportion, uniformly stirring, and standing for 5 minutes to form putty paste; the putty sample (putty paste) which does not need to be pretreated directly proceeds to step S1.
It should be noted that the putty sample may be putty powder or putty paste, when the putty powder is selected as the putty sample, water is added according to a specified proportion, and the putty powder is uniformly stirred and stands for 5 minutes to form the putty paste; when the putty sample is putty paste, the process directly proceeds to step S2.
Preferably, a newly-prepared putty sample (a putty powder and water sample or a putty paste) is directly sampled by a knife adjustment method and is sampled by a sleeve method, wherein the inner diameter of the sleeve is 24mm, and the height of the sleeve is 32/16 mm.
Preferably, step S1 includes laying a putty sample of a specified mass in a parallel plate testing system of a rotational rheometer with a spatula, and controlling the putty sample to lay on the lower plate through the extrusion of the upper plate and contact the edge of the lower plate without forming an extrusion.
Preferably, step S1 includes accurately weighing 8-15 g of putty sample as a test sample, spreading the sample with specified mass in a parallel plate test system of a rotational rheometer by using a knife, keeping the temperatures of an upper plate and a lower plate of the parallel plate test system constant at any temperature within a specified temperature range, lowering the upper plate after the temperature of the putty sample enters the specified temperature range, wherein the downward moving speed of the upper plate is 2mm/S before the gap between the upper plate and the lower plate is greater than 10mm, and after the gap between the upper plate and the lower plate is less than or equal to 10mm, the lowering speed of the upper plate is gradually reduced in a logarithmic mode, and the lowering speed of the upper plate is reduced to zero when the gap value is specified;
preferably, the diameter of a lower plate of the parallel plate test system is 55-65 mm, and the diameter of an upper plate of the parallel plate test system is 50 mm;
preferably, the specified temperature range is 10-35 ℃, and the fluctuation range of the temperature is +/-0.5 ℃.
In the above scheme, the parameter value or parameter range of each datum is the preferred parameter value or parameter range summarized in a large number of experiments by the inventor, and the result obtained by performing the experiments in the range is more accurate.
Preferably, step S2 includes a first test phase and a second test phase which are executed in sequence; wherein, the first test stage is as follows: the shear rate increased linearly from zero to the end of the specified shear rate, and the second test phase was: the shear rate is linearly reduced from the specified shear rate to zero, torque and rotational speed signals are collected at intervals Δ t in each phase, and corresponding shear stress-shear rate data points are calculated and output.
Preferably, the maximum value of the specified shear rate is 10-500 s-1The range of any value, the shearing time of each stage is 0-60 s, and the thickness of the putty sample is 0.5-2 mm.
In the above scheme, the shear rate and the shear time are also the preferable parameter values or parameter ranges summarized in a large number of experiments by the inventor, and the results obtained by performing the experiments in the range are more accurate, and the parameters of the shear rate and the shear time are summarized for the rotational rheometer. The inventor proves in a large number of experiments that when the maximum shear rate is too low or too high, the shear time is too short or too long, the obtained data can not reflect the construction performance, and the data obtained by the too high shear rate has severe fluctuation, so that the repeatability of the data of the plastic viscosity and the yield stress obtained by fitting a flow model is poor. In order to reduce fluctuation and improve data repeatability, the invention provides a baffle structure arranged on the periphery of a lower plate of a parallel plate of a rotational rheometer for limiting edge fracture of a putty sample under high-speed shearing so as to help realize the purposes of reducing fluctuation and improving data repeatability.
Preferably, in step S3, the yield stress and plastic viscosity of the putty sample are obtained by performing a linear fitting process using the Bingham model.
Wherein, the linear fitting treatment by adopting the Bingham model comprises the following steps: fitting effective data points of shear stress-shear rate at which the shear rate is reduced from the specified shear rate to zero, wherein the obtained intercept and slope are respectively the yield stress and the plastic viscosity of the corresponding putty sample;
preferably, the effective data point is that the shear rate is more than or equal to 2s-1All data points of (a).
Preferably, in the step S4, the construction performance of each putty sample is manually scored, and according to the scoring value of each putty sample, the rheological parameter range of each putty sample with the scoring value higher than the set value is selected as the rheological parameter range of the putty construction performance up to the standard.
By adopting the technical scheme, the invention has the following beneficial effects:
1. in the prior art, in the process of testing a putty sample, under a high shear rate, data obtained by a testing device commonly used in the industry has the defects of serious fluctuation, low fitting index, poor repeatability and the like.
2. The method for obtaining the rheological parameter range of the putty is beneficial to guiding the adjustment work of the formula of the putty product from the microcosmic composition structure, provides the rheological parameter range of the excellent putty product with qualified construction hand feeling, and simultaneously can be used as the quality control index of the putty product to replace the subjective scoring method to a certain extent.
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the invention without limiting the invention to its proper form. It is obvious that the drawings in the following description are only some embodiments, and that for a person skilled in the art, other drawings can be derived from them without inventive effort. In the drawings:
FIG. 1 is a schematic diagram of establishing three-dimensional coordinates in an embodiment;
FIG. 2 is a schematic diagram of a selected rheological parameter range;
FIG. 3 is a graph of yield stress versus powder-to-water ratio for the fourth example;
FIG. 4 is a graph of plastic viscosity versus powder-to-water ratio for the fourth example;
FIG. 5 is a step diagram of a method for obtaining the range of rheological parameters of putty in accordance with the present invention.
It should be noted that the drawings and the description are not intended to limit the scope of the inventive concept in any way, but to illustrate it by a person skilled in the art with reference to specific embodiments.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and the following embodiments are used for illustrating the present invention and are not intended to limit the scope of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inside", "outside", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted" and "connected" are to be interpreted broadly, e.g., as being either fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; may be directly connected or indirectly connected through an intermediate. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
The invention provides a method for acquiring rheological parameter range of wall putty construction. Two important rheological parameters of the putty were determined using a cyclic shear test method with a rotational rheometer: yield stress and plastic viscosity, the conditions of cyclic shear are: the shear rate is from 0 to 10 to 0 to 500s-1The shearing time is from 0 to 60s, and the thickness of the sample is 0.5 to 2 mm. By adjusting the formulation of the putty or putty paste, such as the addition of water or cellulose ether, wall putties with different batch scraping hand feeling and rheological property can be obtained. And (3) correlating the hand feeling manual scoring score with the two rheological parameters in the same graph so as to determine the rheological parameter range of the putty product with excellent batch scraping hand feeling.
Example one
The embodiment provides a method for acquiring rheological parameter range of wall putty construction, which is characterized by comprising the following steps:
s1, sampling the putty sample according to the sampling requirement of the rotational rheometer and loading the putty sample;
s2, rheology test: standing the putty sample for 2min, starting testing, collecting a plurality of torque and corresponding rotating speed signals, and respectively calculating and outputting shear stress-shear rate data points;
s3, carrying out data processing on the shear stress-shear rate data points obtained in the step S2 to obtain rheological parameters of the putty sample, wherein the rheological parameters comprise yield stress and plastic viscosity;
s4, obtaining rheological parameters of a plurality of putty samples according to the steps S1-S3, and selecting a rheological parameter range with the putty construction performance reaching the standard according to the construction performance of each putty sample.
Preferably, before step S1, the method further includes a process of pre-treating the putty sample: adding water into the putty sample according to a specified proportion, uniformly stirring, and standing for 5 minutes to form putty paste; wherein, the putty sample without pretreatment directly goes to step S1.
It should be noted that the putty sample may be putty powder or putty paste, when the putty powder is selected as the putty sample, water is added according to a specified proportion, and the putty powder is uniformly stirred and stands for 5 minutes to form the putty paste; when the putty sample is putty paste, the process directly proceeds to step S2.
Preferably, a fresh sample of putty is taken directly by knife adjustment and by the sleeve method, the sleeve has an internal diameter of 24mm and a height of 32/16 mm.
Preferably, step S1 includes laying a putty sample of a specified mass in a parallel plate testing system of a rotational rheometer with a spatula, and controlling the putty sample to lay on the lower plate through the extrusion of the upper plate and contact the edge of the lower plate without forming an extrusion.
Preferably, step S1 includes accurately weighing 8-15 g of putty sample as a test sample, spreading the sample with specified mass in a parallel plate test system of a rotational rheometer by using a knife, keeping the temperatures of an upper plate and a lower plate of the parallel plate test system constant at any temperature within a specified temperature range, lowering the upper plate after the temperature of the putty sample enters the specified temperature range, wherein the downward moving speed of the upper plate is 2mm/S before the gap between the upper plate and the lower plate is greater than 10mm, and after the gap between the upper plate and the lower plate is less than or equal to 10mm, the lowering speed of the upper plate is gradually reduced in a logarithmic mode, and the lowering speed of the upper plate is reduced to zero when the gap value is specified;
preferably, the diameter of a lower plate of the parallel plate test system is 55-65 mm, and the diameter of an upper plate of the parallel plate test system is 50 mm;
preferably, the specified temperature range is 10-35 ℃, and the fluctuation range of the temperature is +/-0.5 ℃.
In the above scheme, the parameter value or parameter range of each datum is the preferred parameter value or parameter range summarized in a large number of experiments by the inventor, and the result obtained by performing the experiments in the range is more accurate.
Preferably, step S2 includes a first test phase and a second test phase which are executed in sequence; wherein, the first test stage is as follows: the shear rate increased linearly from zero to the end of the specified shear rate, and the second test phase was: the shear rate is linearly reduced from the specified shear rate to zero, torque and rotational speed signals are collected at intervals Δ t in each phase, and corresponding shear stress-shear rate data points are calculated and output.
Preferably, the maximum value of the specified shear rate is 10-500 s-1The range of any value, the shearing time of each stage is 0-60 s, and the thickness of the putty sample is 0.5-2 mm.
In the above scheme, the shear rate and the shear time are also the preferable parameter values or parameter ranges summarized in a large number of experiments by the inventor, and the results obtained by performing the experiments in the range are more accurate, and the parameters of the shear rate and the shear time are summarized for the rotational rheometer. The inventor proves in a large number of experiments that when the maximum shear rate is too low or too high, the shear time is too short or too long, the obtained data can not reflect the construction performance, and the data obtained by the too high shear rate has severe fluctuation, so that the repeatability of the data of the plastic viscosity and the yield stress obtained by fitting a flow model is poor. In order to reduce fluctuation and improve data repeatability, the invention provides a baffle structure arranged on the periphery of a lower plate of a parallel plate of a rotational rheometer for limiting edge fracture of a putty sample under high-speed shearing so as to help realize the purposes of reducing fluctuation and improving data repeatability.
Preferably, in step S3, the yield stress and plastic viscosity of the putty sample are obtained by performing a linear fitting process using the Bingham model.
Wherein, the linear fitting treatment by adopting the Bingham model comprises the following steps: fitting effective data points of shear stress-shear rate at which the shear rate is reduced from the specified shear rate to zero, wherein the obtained intercept and slope are respectively the yield stress and the plastic viscosity of the corresponding putty sample;
preferably, the effective data point is that the shear rate is more than or equal to 2s-1All data points of (a).
Preferably, in the step S4, the construction performance of each putty sample is manually scored, and according to the scoring value of each putty sample, the rheological parameter range of each putty sample with the scoring value higher than the set value is selected as the rheological parameter range of the putty construction performance up to the standard.
Example two
The second embodiment provides a method for obtaining the rheological parameter range of wall putty construction, which comprises the following steps: and measuring rheological parameters of a plurality of putty samples, manually scoring the construction performance of each putty sample, and determining the range of the rheological parameters of which the putty construction performance reaches the standard according to the scoring value of each putty sample.
In the scheme, the acquisition of the rheological parameter range of the putty construction performance up to the standard is based on manual scoring, and the accuracy of the rheological parameter range of the putty construction performance up to the standard can be improved by scoring the putty sample by qualified constructors. If the construction performance is judged by a constructor all the time, the judgment result is easily influenced by personal subjective factors, and the grading results given by different persons or even the same person at different time are possibly inconsistent, so that the uncertainty of the grading result caused by the inconsistency of the subjective human factors interferes the development work of the product formula to a great extent, and in the aspect of controlling the quality stability of the delivered product, a set of objective and reliable technical indexes is urgently needed to measure the batch scraping hand feeling of the putty product. The construction performance of the putty product can be judged according to the relationship between the rheological parameters of the putty product and the rheological parameter range of the putty construction performance up to the standard, which is determined by the method, and the objective and unified quality management of a factory is facilitated.
Preferably, the rheological parameters of the putty samples comprise two parameters of yield stress and plastic viscosity, and the parameter range of the yield stress and the plastic viscosity of each putty sample with the score value higher than a set value is used as the rheological parameter range of the putty construction performance up to the standard. Generally, the construction hand feeling and the rheological property of the putty are related, the smaller the two rheological parameters are, the better the hand feeling is, but when the rheological parameters are too small, the putty can sag, and the construction quality is influenced.
Preferably, the rheological parameter range for determining the up-to-standard putty workability comprises the following steps: establishing a two-dimensional coordinate system by taking yield stress and plastic viscosity as X-Y coordinate axis variables, drawing rheological parameter information of each putty sample in the two-dimensional coordinate system, and performing range selection on each data point with a score higher than a set value in a plane of the two-dimensional coordinate to obtain a rheological parameter range with the standard putty construction performance;
or, referring to fig. 1, the rheological parameter range for determining the up-to-standard putty workability includes: and respectively establishing a three-dimensional coordinate system by using the yield stress, the plastic viscosity and the manual score as X-Y-Z coordinate axis variables, drawing three variable data of each putty sample in the three-dimensional coordinate system, selecting each putty sample with the manual score higher than a set value in the Z axis to project to an X-Y plane, and performing range selection on each data point projected on the X-Y plane to obtain the rheological parameter range with the standard putty construction performance.
Preferably, referring to fig. 2, the range of rheological parameters within which the putty workability reaches the standard is obtained by selecting each data point higher than a set value in the X-Y plane by using a rectangular frame, or is a selected range obtained by connecting each boundary point of each data point set higher than the set value in the X-Y plane in sequence by lines.
In the scheme, the line is sequentially connected with each boundary point of each data point set which is higher than the set value in the X-Y plane to obtain the selection range of the irregular figure shape, and the selection range of the irregular figure is more accurate.
Preferably, the rheological parameter range for the up-to-standard putty construction performance comprises a first rheological parameter range for selecting all data points with manual scores higher than a set value in an X-Y plane and a second rheological parameter range for further selecting an area with densely distributed data points in the first rheological parameter range.
In the scheme, the small parameter range with densely distributed data points is selected in the first rheological parameter range in a large range, so that the design of a putty component formula is guided, the putty component is prepared in the second rheological parameter range, the construction performance of a putty product can be ensured, and when the rheological parameter of the putty product falls in the second rheological parameter range, the probability that the construction performance of the putty product reaches the standard can be increased.
Preferably, after the rheological parameter range of the putty construction performance up to the standard is determined, the method also comprises a process of correcting the rheological parameter range.
In the above solution, a more accurate rheological parameter range can be obtained by modifying the rheological parameter, and a modification method is provided as follows:
s101, respectively dividing yield stress, plastic viscosity and manual grading into X-Y-Z coordinate axis variables to establish a three-dimensional coordinate system, and drawing three variable data of each putty sample in the three-dimensional coordinate system;
s102, projecting data points of each putty sample with the manual score higher than a set value in a Z axis to an X-Y plane, and performing range selection on the data points projected on the X-Y plane to obtain a rheological parameter range with the putty construction performance up to the standard;
s103, projecting data points of each putty sample with the manual score lower than the set value to an X-Y plane, and performing range selection on each data point with the manual score lower than the set value projected on the X-Y plane to obtain a rheological parameter range with the putty construction performance not reaching the standard;
wherein, the range of the rheological parameter of which the putty construction performance does not reach the standard obtained in the step S103 and the range of the rheological parameter of which the putty construction performance reaches the standard obtained in the step S102 have intersection;
and S104, deleting the intersection part of the range of the rheological parameters which reach the standard of the putty construction performance obtained in the step S102 and the range of the rheological parameters which do not reach the standard of the putty construction performance obtained in the step S103, thereby obtaining a more accurate range of the rheological parameters which reach the standard of the putty construction performance.
Preferably, in order to further improve the correction effect, the construction performance of the putty sample is divided into multiple grades, each grade of putty sample is projected to an X-Y plane to obtain multiple rheological parameter ranges, the multiple rheological parameter ranges comprise a plurality of rheological parameter ranges with standard construction performance and a plurality of rheological parameter ranges with substandard construction performance, the rheological parameter ranges have intersection, and when the rheological parameter range of a certain grade of putty sample is to be obtained, the intersection area of the certain grade of putty sample and other grade of putty samples is deleted in the rheological parameter range of the certain grade of putty sample, so that a more accurate putty parameter range can be obtained.
For example:
the construction performance of the putty is graded into 0 to 3 by the senior constructor, and the grading system is as follows:
the method has the advantages that: 2.3-2.5 min;
good: 2.1-2.3 min;
medium: 2.0 min;
difference: less than 2.0 min;
when obtaining the range of the rheological parameters of the putty sample with excellent score, respectively projecting the putty sample with each grade to an X-Y plane to obtain four ranges of the rheological parameters of the putty, wherein the edges of the four ranges of the rheological parameters of the putty have intersection, and for conservation, the intersection part of the four ranges of the rheological parameters of the putty sample with other three ranges needs to be deleted. In essence, the range of rheological parameters of the intersecting putty is a transition range, and the putty with rheological parameters in the transition range has great uncertainty on the workability, so the range is preferably deleted.
In the scheme, the obtained rheological parameter range of the putty construction performance up to the standard is obtained by testing limited putty samples, so that in order to improve the accuracy of the rheological parameter range of the putty construction performance up to the standard, the correcting process also comprises the step of continuing to test more putty samples in the subsequent process, thereby correcting the previously determined rheological parameter range.
Preferably, the construction performance of the putty sample comprises batch scraping hand feeling during construction;
preferably, the highest score is set for the construction performance of the putty samples, and the rheological parameter range of each putty sample with the construction performance score of more than 70 percent of the highest score is obtained and is the rheological parameter range with the standard putty construction performance.
Preferably, determining the rheological parameters of the putty sample comprises the following steps:
s1, sample pretreatment: adding water into the putty sample according to a specified proportion, uniformly stirring, and standing for 5 minutes to form putty paste; wherein, the step S2 is directly proceeded without the sample pretreatment;
s2, sampling the putty paste according to the sampling requirement of the rotational rheometer and loading the samples: flatly spreading putty paste with specified mass in a parallel plate testing system of a rotational rheometer by using a knife, controlling the putty paste to be flatly spread on a lower plate through the extrusion of an upper plate, and contacting the edge of the lower plate without forming extrusion;
s3, rheology test: the sample putty paste starts to be tested after standing for 2min, and the first stage is sequentially executed: the shear rate is linearly increased from zero to the end of the specified shear rate, and the second stage: linearly reducing the shear rate to zero from the specified shear rate, acquiring torque and rotating speed signals at intervals of time delta t in each stage, and calculating and outputting corresponding shear stress-shear rate data points;
and S4, performing linear fitting treatment on the shear stress-shear rate data points obtained in the step S3 to obtain the yield stress and the plastic viscosity of the putty sample.
Preferably, in step S4, a Bingham model is used to perform a linear fitting process to fit valid data points of shear stress-shear rate where the shear rate decreases from the specified shear rate to zero, and the resulting intercept and slope are the yield stress and plastic viscosity of the corresponding putty sample, respectively;
preferably, the effective data point is that the shear rate is more than or equal to 2s-1All data points of the range.
Preferably, in step S3, the maximum value of the specified shear rate is 10-500S-1The range of any value, the shearing time of each stage is 0-60 s, and the thickness of the putty sample is 0.5-2 mm.
In the prior art, in the testing process of the putty sample, under the condition of high shear rate, data obtained by a testing device commonly used in the industry has the defects of serious fluctuation, low fitting index, poor repeatability and the like.
EXAMPLE III
In the third embodiment, a specific method for obtaining the range of the rheological parameter is provided according to a specific example:
step one, preparing a putty paste sample according to the formula in table 1.
The sample preparation method comprises the following steps: adding a proper amount of water into a kettle for production, slowly adding the adhesive while stirring by a dispersion disc at a constant speed, sequentially adding other auxiliaries such as a defoaming agent and the like to generate a large amount of foams, and obtaining uniform dispersion liquid after 15 min. Slowly adding heavy calcium powder, reducing the rotation speed of a dispersion disc, and dispersing for 15min to obtain a paste finished product.
Table 1 base formulation composition of surface layer putty samples
And step two, collecting a sample at the lower part of the kettle, and filling the sample into a 5L tank. Samples for batch scraping, rheology, bench jump and consistency testing were taken with tools in the same 5L tank.
And step three, performing rheological test on the putty paste sample. The lower plate of the rheometer is adjusted to a constant temperature, 12.2g of putty paste sample with specified mass is placed at the central position of the lower plate of the rotational rheometer by using an adjusting knife, the distance between the upper plate and the lower plate (the thickness of the sample) is slowly reduced to 1mm according to a preset program, and the sample is kept still for 120s so as to completely eliminate the internal temperature difference. After the test started, the upper plate applied the specified program of continuous horizontal shear to the sample, first stage: shear rate from 0s-1To 500s-1And a second stage: the shear rate is further from 500s-1Decrease by 0s-1. For the second segment, 15 data points are taken, 1-12 points are selected and fitted by a Bingham fluid model to obtain the yield stress and the plastic viscosity. In total, 6 replicates were taken. And performing linear fitting treatment on each test result to obtain an intercept and a slope which are the yield stress and the plastic viscosity of the sample respectively. The results of the treatment are shown in Table 2.
TABLE 2 rheological parameter Table after fitting
The data in table 2 were processed by statistical method to obtain an average value of yield stress of 562Pa and a relative standard deviation of 5.7%; the average plastic viscosity was 8.6Pa-s and the relative standard deviation was 2.7%. The statistical average of the yield stress and plastic viscosity are filled in table 3 below.
And step four, measuring and evaluating other samples in the table 1 by the methods of the step one, the step two and the step three to obtain the results in the table 3.
TABLE 3 rheological parameters and conventional workability test data for multiple putty paste samples
And step five, as shown in figure 1, establishing a three-dimensional coordinate system by respectively dividing the yield stress, the plastic viscosity and the manual score into X-Y-Z coordinate axis variables, drawing three variable data of each putty sample in the three-dimensional coordinate system, selecting putty sample data points with the score of more than 2.1 in the table 3 to project to an X-Y plane, as shown in figure 2, and selecting each data point in the X-Y plane by adopting a rectangular frame to obtain the rheological parameter range with the standard putty construction performance.
Example four
The implementation provides that the consistency of the result obtained by the method and the subjective scoring result is verified by adding water to a soapy fruit sample
The three putty powders are respectively expressed by Z, B and M codes.
Wherein the subjective scoring result is as follows:
when the water-powder ratio (water to putty sample) is 1:2.6, the construction hand feeling order is Z < B ≈ M
When the water-powder ratio is 1:2.9, the construction hand feeling is ordered that B is less than M and less than Z
The results of the rheological test are:
when the water-powder ratio is 1:2.6, the yield stress M is less than B and less than Z, the plastic viscosity B is less than M and less than Z
When the water-powder ratio is 1:2.9, the yield stress B is less than M and less than Z, the plastic viscosity B is less than M and less than Z
TABLE 4 construction hand feel scoring results for three putty water-blended samples at two water-powder ratio formulas
TABLE 5 rheology parameters of three putty powder blended water samples at six water-to-powder ratio formulations
A graph of rheological parameters versus powder to water ratio is plotted according to the data in table 5: see fig. 3 and 4.
In the invention, the consistency data is according to the Chinese national standard GB/T1749-79 'Thick paint, putty consistency test method'. The data of the jumping table refer to GB/T2419-2005 'Cement mortar fluidity acquisition method', the used test mold is a cylinder with a smooth inner wall, the inner diameter of the cylinder is 32mm, and the height of the cylinder is 32 mm. The spread diameter of the putty sample was recorded immediately after shaking the table up and down 15 times.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (12)
1. A method for acquiring a rheological parameter range of wall putty construction is characterized by comprising the following steps:
s1, sampling the putty sample according to the sampling requirement of the rotational rheometer and loading the putty sample;
s2, rheology test: standing the putty sample for 2min, and then starting testing, wherein the testing comprises a first testing stage and a second testing stage which are sequentially executed; wherein, the first test stage is as follows: the shear rate increased linearly from zero to the end of the specified shear rate, and the second test phase was: linearly reducing the shear rate to zero from the specified shear rate, acquiring torque and rotating speed signals at intervals of time delta t in each stage, and calculating and outputting corresponding shear stress-shear rate data points;
s3, carrying out data processing on the shear stress-shear rate data points obtained in the step S2 to obtain rheological parameters of the putty sample, wherein the rheological parameters comprise yield stress and plastic viscosity;
s4, obtaining rheological parameters of a plurality of putty samples according to the steps S1-S3, manually scoring the construction performance of the putty samples, and associating hand feeling manual scoring scores with the two rheological parameters in the same graph so as to determine the range of the rheological parameters of the putty products with excellent batch scraping hand feeling.
2. The method for obtaining the rheological parameter range of the wall putty construction, which is characterized by further comprising the following steps of preprocessing a putty sample before the step S1: adding water into the putty sample according to a specified proportion, uniformly stirring, and standing for 5 minutes to form putty paste; wherein, the putty sample without pretreatment directly goes to step S1.
3. The method for obtaining the rheological parameter range of wall putty construction, which is characterized in that a newly-prepared putty sample is directly sampled by a knife adjustment method and is sampled by a sleeve method, wherein the inner diameter of the sleeve is 24mm, and the height of the sleeve is 32/16 mm.
4. The method of claim 1, wherein step S1 comprises placing a sample of putty of a given mass in a parallel plate test system of a rotational rheometer, and controlling the sample of putty to be placed on the lower plate by the upper plate pressing and to contact the edge of the lower plate without forming a press.
5. The method for obtaining the rheological parameter range of the wall putty construction of any one of claims 1 to 4, characterized in that step S1 includes accurately weighing 8-15 g of putty sample as a test sample, flatly paving the sample with specified mass in a parallel plate test system of a rotary rheometer, keeping the temperature of an upper plate and a lower plate of the parallel plate test system at any temperature within a specified temperature range, descending the upper plate after the temperature of the putty sample enters the specified temperature range, ensuring the downward moving speed of the upper plate to be 2mm/S before the gap between the upper plate and the lower plate is larger than 10mm, gradually reducing the descending speed of the upper plate in a logarithmic mode after the gap between the upper plate and the lower plate is smaller than 10mm, and reducing the descending speed of the upper plate to zero when the gap value is specified.
6. The method for obtaining the rheological parameter range of wall putty construction, which is characterized in that the diameter of a lower plate of a parallel plate testing system is a 55-65 mm circular plate, and the diameter of an upper plate of the parallel plate testing system is a 50mm circular plate.
7. The method for obtaining the rheological parameter range of the wall putty construction, which is characterized in that the specified temperature range is 10-35 ℃, and the fluctuation range of the temperature is +/-0.5 ℃.
8. The method for obtaining the rheological parameter range of wall putty construction, which is characterized in that the maximum value of the specified shear rate is 10-500 s-1The range of any value, the shearing time of each stage is 0-60 s, and the thickness of the putty sample is 0.5-2 mm.
9. The method for obtaining the rheological parameter range of the wall putty construction, which is characterized in that in the step S3, a Bingham model is adopted to perform linear fitting treatment to obtain the yield stress and the plastic viscosity of a putty sample.
10. The method for acquiring the rheological parameter range of the wall putty construction, which is characterized in that the Bingham model is adopted for linear fitting treatment, and the method comprises the following steps: fitting valid data points of shear stress-shear rate where the shear rate decreases from the specified shear rate to zero, the resulting intercept and slope are the yield stress and plastic viscosity, respectively, of the corresponding putty sample.
11. The method for obtaining the rheological parameter range of wall putty construction as claimed in claim 10, wherein the effective data point is that the shear rate is not less than 2s-1All data points of (a).
12. The method for obtaining the rheological parameter range of the wall putty construction of claim 1, wherein in step S4, the method comprises manually scoring the construction performance of each putty sample, and selecting the rheological parameter range of each putty sample with the score value higher than a set value as the rheological parameter range of the putty construction performance up to the standard according to the score value of each putty sample.
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| WO2017059323A1 (en) * | 2015-10-01 | 2017-04-06 | Ecolab Usa Inc. | Method for simulating high pressure paraffinic froth treatments |
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| CN102393348A (en) * | 2011-10-26 | 2012-03-28 | 常州天合光能有限公司 | Method for testing rheological property of conductive slurry |
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