The above study shows that the floor of working face II633 is damaged to a greater depth under the influence of mining disturbance and the coupling effect of the confined water. The confined water is likely to break through the key stratum of the aquiclude through the confined water conduction zone and conduct with the mining damage zone, which will cause a floor water inrush accident, and the risk of floor water inrush is large. For this reason, the coal seam floor needs to be reinforced by grouting to reduce the depth of damage to the floor and to reduce the risk of water inrush from the floor. To achieve the ideal grouting effect, in addition to the excellent grouting process, the ratio and performance of the slurry material are also crucial to the grouting effect. In this section, bentonite, a water–reducing agent, and sodium silicate were selected as slurry additives, the water cement ratio, viscosity, setting time, and compressive strength of the slurry were used as slurry performance evaluation indexes, and a single factor test was adopted to determine the optimal selection range of the slurry content, and the response surface optimization analysis method was adopted to determine the optimal value of each index.
4.1. Selection of Grouting Materials and Performance Index
The research found that bentonite can improve the water separating proportion of the cement slurry and improve the stability of the slurry, the water–reducing agent can reduce the viscosity of the cement slurry and improve the plasticity of the cement slurry, and sodium silicate can effectively shorten the setting time of the cement slurry. Therefore, this paper drew on the experience of road construction, mixed the above–mentioned materials into the grouting materials, and achieved the purpose of ensuring the grouting effect, reducing the cost of grouting, and increasing the profit of tons of coal by optimizing the ratio of each material.
- (1)
Bentonite properties
Bentonite is a yellow–green clay that is easy to swell for paste after adding water; it has a low permeability and can effectively improve the slurry water separating proportion. Its main component is montmorillonite (80~90%), and the PH value is between 8.9 and 10, containing more active metal cations such as Cu2+, Mg2+, Na+, and K+, etc., and has superior ion exchange properties.
According to the interlayer cations, bentonite can be classified into Na–bentonite, calcium–based bentonite, hydrogen–based bentonite, and organic bentonite. Na–bentonite was selected for this experiment, and its physical parameters are shown in
Table 1.
- (2)
Water–reducing agent properties
The water–reducing agent is an anionic surfactant, and it can interact with the cations in the cement hydration products; the reaction product is cross–linked adsorbed on the surface of the cement particles within a certain period of time to hinder or destroy the adsorption cohesion between the cement particles. The selected high–efficiency water–reducing agent from the naphthalene series water–reducing agent has the appearance of a yellow to dark brown powder and is easily soluble in water. Adding a water–reducing agent to concrete can not only increase the strength but also improve its wear resistance, corrosion resistance, and resistance to permeability; its physical properties are shown in
Table 2.
- (3)
Sodium silicate properties
Sodium silicate, a soluble inorganic silicate, is an aqueous solution of sodium silicate (chemical formula Na2O·nSiO2), which is widely used as a mining binder. For the cement slurry with sodium silicate, sodium silicate has a catalytic effect on cement hydration, the cement slurry contains calcium hydroxide, and sodium silicate reacts with it to generate hydrated calcium silicate (hydrated calcium silicate is a kind of cementitious body, and it has high strength) while consuming a certain amount of calcium hydroxide so that its content cannot reach saturation, thus accelerating the hydration of calcium silicate, improving the initial setting time of the cement slurry and increasing the early compressive strength of the grouting stone body. In addition, the charge carried by the slurry colloid is opposite to the charge carried by the sodium silicate, and the two have opposite electrical properties, which can effectively improve the setting speed of the slurry after the neutralization and condensation of the colloidal particles.
4.2. Slurry Performance Index Test
The performance indexes of the slurry injection slurry for water plugging and reinforcing the floor rock, excluding the cost of slurry injection, also need to consider the performance indexes of the slurry itself, including the slurry water separating proportion, viscosity, setting time, and the compressive strength of the grouting stone body [
42].
- (1)
Determination of slurry water separating proportion
The slurry water separating proportion refers to the volume ratio of water separation from the slurry at rest due to the natural settlement of cement particles by gravity, which is one of the important indicators to measure the stability of the slurry and the degree of fracture filling. To determine the water separating proportion, the configuration of the slurry poured into the cylinder, the liquid level, and the 1000 mL scale value flush, the mouth of the cylinder was sealed, placed on the horizontal table, and rested for 3 h for every 10 mine observation and the data were recorded; three consecutive readings of the same can be identified as the slurry was completely water separated to achieve stability. When testing another slurry water separating proportion, the cylinder should be cleaned and kept dry inside.
- (2)
Slurry viscosity measurement
The slurry viscosity is a physical quantity that measures the internal friction of a slurry as it flows, and it represents the rheology and injectability of the slurry. In this experiment, a funnel viscometer was selected for the viscosity determination by the time required for a unit volume of the slurry to flow out of the lower port of the funnel.
- (3)
Slurry setting time measurement
For the slurry setting time for each slurry admixture hydration reaction time required, there is an initial setting, a final setting time, and the test selection of the Vicat instrument for slurry setting time determination. For the determination of the initial setting time when the initial setting needle from the bottom of the test mold 4 mm ± 1 mm can be for the slurry beginning the initial setting. For the determination of the final setting time, the final setting needle and then the test mold surface does not leave a ring–shaped imprint shall prevail.
- (4)
Determination of the compressive strength of the grouting stone body
The slurry condensed to form a stone body, and the compressive strength is the stone strength, which visually reflects the bearing capacity of the reinforced rock formation. The mixed slurry with different admixture ratios was poured into a standard mold of 50 mm × 100 mm to make standard specimens, and after the time condensation and demolding, it was placed into a standard curing box and cured for 7 d and 28 d, respectively, to test the compressive strength of the specimens. Each slurry performance index measurement test is shown in
Figure 4.
4.3. Single–Factor Experimental Design and Result Analysis of Grouting Material Proportioning
- (1)
The effect of single admixture addition on slurry performance
- (a)
The effect of different water–cement ratio on slurry performance
According to the ⟪Specification of mine curtain grouting⟫ [
43,
44,
45], the water–cement ratios selected for this single–factor experiment ranged from 0.5, 0.6, 0.8, 1.0, and 2.0. After the slurry was completely mixed, the water separating proportion, viscosity, setting time, and compressive strength of the grouting stone body of the slurry were measured under different water–cement ratios, and the test results are shown in
Figure 5.
From the analysis of
Figure 5, it can be seen that: in the water separating proportion, the slurry water separating proportion is closely related to the water–cement ratio. The greater the water–cement ratio, the faster the slurry water separation and the greater the water separating proportion, and when the water–cement ratio is 0.6, the slurry water separating proportion is stable at 6.1% at 150 min, while the water–cement ratio is 2.0, the slurry water separating proportion is stable at 52% at 90 min, the slurry performance is greatly reduced. In terms of viscosity, the viscosity of slurry decreases with the increase in the water–cement ratio value, and they are negatively correlated; the viscosity decrease values are 489.6 s, 28.8 s, 9.5 s, and 1.9 s during the increase in the water–cement ratio from 0.5 to 2.0, the viscosity decrease values are 489.6 s, 28.8 s, 9.5 s, and 1.9 s. When the water–cement ratio value increases from 0.6 to 0.8, the viscosity decrease is larger, i.e., the slurry is less liquid and unfavorable for grouting when the water–cement ratio is larger. In terms of setting time, the trend of the initial and final setting time of the slurry is that the setting time gradually increases with the increase in the water–cement ratio, and when the water–cement ratio is 2.0, the final setting time can reach 23.4 h. This is because the larger the water–cement ratio, the freer the water in the slurry, and the greater the effect of dissolving and dispersing the colloid and crystal of the slurry after hydration, which directly leads to the longer setting time of the slurry; in terms of compressive strength of the grouting stone body, its overall trend when the water–cement ratio is 2.0, the compressive strength of the grouting stone body at 28d is only 16.3 MPa, which is lower than the standard of compressive strength of the grouting stone body not less than 17 MPa required in the grouting project, because the larger the water–cement ratio, the freer the water in the slurry, and the water evaporates after the slurry solidifies, the stone body will form microscopic pores inside the slurry. The freer the water, the greater the porosity, which seriously affects the compressive strength of the grouting stone body. Therefore, the water–cement ratio can be selected from 0.6–1.0.
- (b)
Influence of bentonite dosing on slurry performance
To study the effect of bentonite dosing on the slurry performance, the fixed water–cement ratio was 0.8, the water–reducing agent and sodium silicate dosing were 0.4% and 1%, respectively, and the bentonite dosing was set at four gradients of 1%, 2%, 3%, and 4%. It is necessary to soak the bentonite and water in the container in a ratio of 1:1 for more than 48 h to produce flocculation. The water separating proportion, viscosity, coagulation time, and compressive strength of the grouting stone body of the slurry under different bentonite doping were measured separately, and the experimental results are shown in
Figure 6.
The analysis from
Figure 6 can be obtained: in the water separating proportion, the greater the amount of bentonite, the slurry water separating proportion reduction trend, the better the stability of the slurry, and all within 80 min water separation stability, that is, bentonite can significantly inhibit the slurry water separating proportion. In the slurry viscosity, the greater the bentonite doping, the greater the viscosity of the slurry, dosing from 1% to 3%, the viscosity of the slurry from 24.2 s to 29.5 s, an increase of 5.36 s, and from 3% to 4%, the viscosity of the slurry from 29.5 s to 50.2 s, and an increase of 20.7 s, which is due to the high concentration of Na
+ in the slurry, can be to due the large number of anions it combined with. The moisture absorption effect is obvious, but the slurry viscosity required in the grouting project needs to be less than 40 s, so bentonite dosing does not take 4%; in the setting time and compressive strength of the grouting stone body, bentonite dosing on the initial setting of the slurry, the final setting time has a certain delayed effect, while the strength after 7 d, 28 d maintenance is slightly weakened, but from an overall view, bentonite dosing on the two slurry performance indicators has very little effect, in the project can be ignored, so the bentonite dosing range is 1–3%.
- (c)
The effect of water–reducing agent admixture on slurry performance
In order to study the effect of water–reducing agent dosing on the slurry performance, the water–cement ratio was fixed at 0.8, the dosing of bentonite and sodium silicate were fixed at 1%, and the water–reducing agent dosing was set at five gradients of 0.2%, 0.4%, 0.6%, 0.8%, and 1.0%. When the slurry was stabilized, the water separating proportion, viscosity, setting time, and compressive strength of the grouting stone body of the slurry were measured under different water–reducing agent doses, and the experimental results are shown in
Figure 7.
From the analysis of
Figure 7, it can be obtained that: in the water separating proportion, when the water–reducing agent is mixed in the range of 0.2% to 0.8%, the water separating proportion of the slurry increases with the increase in water–reducing agent, and when the water–reducing agent is mixed at 1%, the slurry does not separate water but appears stratified, which is due to the dispersing effect of water–reducing agent on cement hydrate, prompting the dispersion of large and small particles in the slurry, the larger particles sink to the bottom, while the smaller slurry particles are suspended in the upper layer. In terms of slurry viscosity, the viscosity does not change much when the water–reducing agent dosing is 0.2–0.4%, but when the dosing is increased from 0.4% to 0.8%, the viscosity decreases from 24.2 s to 17.4 s, with a decrease rate of 6.8 s. The reduction rate is faster, and the viscosity reduction effect of the water–reducing agent is obvious. In terms of setting time, the water–reducing agent has an inhibiting effect on setting time, especially when the dosing is greater than 0.4%, and the reason for the inhibitory effect is that the anion of the water–reducing agent dissolved in water combined with cement particles to form a thin film layer, which hinders the adsorption and coagulation between the particles. In terms of the compressive strength of the grouting stone body, different water–reducing agents have little effect on the compressive strength of the grouting stone body of the slurry. To sum up, the selection range of water–reducing agent dosing is 0.4–0.8%.
- (d)
The effect of sodium silicate admixture on slurry performance
In order to study the effect of water–glass dosing on the slurry performance, the water–cement ratio was fixed at 0.8, the dosing of bentonite and water–reducing agent were fixed at 1% and 0.4%, respectively, and the water–glass dosing was set at four gradients of 1%, 2%, 3%, and 4%. When the slurry was stabilized, the water separating proportion, viscosity, setting time, and compressive strength of the grouting stone body of the slurry were measured under different sodium silicate dosing, and the visual graph of the experimental results is shown in
Figure 8.
The analysis from
Figure 8 can be obtained: in the water separating proportion, the sodium silicate dosing for the slurry water separating proportion has a significant inhibitory effect; the greater the sodium silicate dosing, the smaller the slurry water separating proportion, the drop gradually decreases, and the drops between the different gradients were 10%, 9%, and 2.5%. The viscosity of the slurry is positively correlated with the amount of sodium silicate; when the amount of sodium silicate is increased from 1% to 4%, the viscosity increases from 24.1 s to 28.1 s, and the increase range is 4 s. In terms of setting time, the water–reducing agent can promote the setting of the slurry, and with the increase in the amount of sodium silicate, the initial and final setting time of the slurry is gradually shortened. In terms of the compressive strength of the grouting stone body, the amount of sodium silicate has a small effect on the strength of the stone body; in summary, it is determined that the selection range of sodium silicate admixture is 1–3%.
4.4. Response Surface Experimental Design of Slurry Proportioning Based on CRITIC Weighting Method
Based on the single–factor experiments affecting the slurry performance, it is also necessary to clarify the interaction relationships among the influencing factors, for which a response surface test design is adopted in this paper to optimize the proportion of grouting materials. The response surface test can determine the correlation between the factors and the corresponding regression equation within a certain test range. Considering the two–by–two interaction between the different influencing factors and single–factor quadratic term influence, this test adopts the second–order response surface model and designs a four–factor, three–level test, and the setup results are shown in
Table 3.
The specific experimental design method was a response surface analysis design using the water–cement ratio (A), bentonite (B), water–reducing agent (C), and sodium silicate (D) as response factors. The Box–Behnken test method in the Design expert software was used to analyze the response to the combined scores of the water separating proportion, viscosity, setting time, and compressive strength, and the test was divided into 29 groups, including 24 groups of precipitation factor tests and five groups of central tests. The test results are shown in
Table 4.
In order to objectively assign weights to each influencing factor, the CRITIC weight method was used in this paper to calculate the influence weights of the water–cement ratio, bentonite dosing, water–reducing agent dosing, and water–glass dosing on slurry performance using the magnitude of data correlation among the factors.
- (1)
Standardization and normalization
The different characteristics of the material have different measurement and reflection laws that need to be standardized and normalized. Among them, according to the actual needs of the floor confined water grouting reinforcement project, set the compressive strength of the grouting stone body and viscosity as the positive indicators; that is, the larger the value, the better the setting time and water separating proportion as the inverse indicators; that is, the hope of small characteristics, the different characteristics of the data normalized distribution according to Formulas (12) and (13) calculations.
where
is the data normalization results;
is the amount of indicators tested in the
jth group of tests;
is the maximum value of the detection amount of each index; and
is the minimum value of the detection amount of each index.
- (2)
Variability of indicators
In the CRITIC method, the standard deviation is used to indicate the fluctuation of the difference in the values taken within each indicator. The larger the standard deviation indicates a greater difference in the value of the indicator, and more information can be reflected, and the stronger the evaluation intensity of the indicator itself, and more weight should be assigned to the indicator.
where
is the Standard deviation of the
jth indicator.
- (3)
Conflicting indicators
The stronger the correlation with other indicators, the less conflicting the indicator is with other indicators, the more the same information is reflected, and the more duplication of the evaluation content is reflected, which to some extent also weakens the evaluation strength of the indicator and should reduce the weight assigned to the indicator.
where
is the number of indicators tested in the
jth group of tests.
- (4)
Amount of information
- (5)
Objective weights
Substituting the test results data in
Table 2 into Equations (15)–(20), the values of each evaluation index can be calculated, as shown in
Table 5. From
Table 5, the weighting of each slurry performance index can be obtained as follows: viscosity > setting time > compressive strength of the grouting stone body > water separating proportion.
In order to obtain the correlation between the evaluation object and the optimal solution, the calculation of the gray correlation coefficient requires setting up a reference sequence and a comparison sequence and performing the calculation of the deviation sequence. The grey correlation coefficient is obtained by taking the water separating proportion, viscosity, setting time, and the compressive strength of the grouting stone body as the comparison sequence and the normalized weighted results of the four indicators as the reference sequence.
where
is the judgment coefficient defined in (0, 1) is taken to be 0.5.
The gray correlations of each group of tests under different properties were taken as the weighted average, as a quantitative expression of the correlation between the reference and comparison sequences, which is the comprehensive evaluation degree
G of the material modification effect, and the larger
G indicates the better comprehensive properties of the material. The results of gray correlation values of different properties and CRITIC weighted comprehensive evaluation are shown in
Table 6.
4.5. Analysis of Comprehensive Evaluation Results
- (1)
Evaluation model establishment
Multiple regressions were fitted to the test data in
Table 2;
Table 4 using Design expert software to establish a composite score response model. The regression equation for the composite score was:
where
y is the composite score response value;
x1 is the water–cement ratio;
x2 is the bentonite dosing;
x3 is the water–reducing agent dosing; and
x4 is the sodium silicate dosing.
The residual normal probability of the model is shown in
Figure 9. As can be seen from
Figure 9, the test points are distributed on the diagonal and on both sides of the diagonal, and the average deviation of the model is small, indicating that the model is reasonably established and the reliability of the fitted equations is good. The residual results of the prediction model are shown in
Figure 10, where the residuals are randomly distributed around zero with no outliers, indicating that the predicted and measured values are in high agreement.
The analysis of variance of the regression equation after fitting the prediction model is shown in
Table 7. From the analysis in
Table 7, it can be concluded that the
p–value of the model is less than 0.01, and the model is extremely significant and statistically significant. For the four single factors, A, B, C, and D, the main order of influence of the four factors is B > C > D > A; that is, the bentonite admixture has the most significant effect on the slurry performance, the water–reducing agent admixture, sodium silicate admixture, and the water–cement ratio is the second. The misfit terms of the models are all greater than 0.05, the misfit is not significant, the experimental error is small, and the fit with the actual law is high.
The results of the model credibility analysis are shown in
Table 8. As can be seen from
Table 8, the correlation coefficient and the modified correlation coefficient of the model are 0.8301 and 0.8603, respectively, which are close to a high degree, indicating that the regression equation is a good fit. The signal-to-noise ratio was 7.566 > 4, while the coefficient of variation was 11.95%, indicating the high precision and credibility of the test.
- (2)
Two–by–two interaction between factors
The response curve diagram represents the response results with two of the factors constituting the three–dimensional graph, the curvature of the response surface represents the degree of interaction between the factors; the curvature is large, indicating that the interaction between the factors has a greater impact and vice versa indicating that the interaction has a smaller impact. In order to analyze the influence of the interaction between the water–cement ratio, silica powder, and liquid alkali on the comprehensive evaluation of the model, the response surface plot of the influence of the interaction between each factor is drawn as shown in
Figure 11.
From the analysis of
Figure 11, to determine the optimal ratio of materials: water–cement ratio 0.808, bentonite 2.326%, water–reducing agent 0.568%, sodium silicate 2.197%, modified water–cement ratio, and each grouting material admixture are water–cement ratio 0.8, bentonite 2%, water–reducing agent 0.6%, and sodium silicate 2%.