4.1. Effect of Using a Single Super Retarder on the Setting Time of Waste Slurry Recycled Water
Seven kinds of super retarders were selected, and the effect of different dosage of super retarders on the setting time of waste slurry recycled water was investigated by external doping method.
Figure 2 shows the effect of 0.5%, 1.0%, 1.5%, 2.0% super retarding agent on the setting time of recycled water, the dosage of super retarding agent is the ratio of the mass of recycled water.
As can be seen in
Figure 2, after using 0.5% of super retarding agents, the four super retarding agents, SDP-90, ACS, PBTCA and HEDP-4Na, can make the slurry recycled water setting time of more than 10 h, compared with the reference group of 7 h, it can be seen that the four super retarding agents 0.5% dosage of the retarding effect of the better. Among them, SDP-90 has the best effect on retardation of slurry recycling water, and the final measurement of the beginning of the setting time is 13 h. However, when using the two super retarders AA/AMPS or IDS, the setting time of the waste slurry recycled water was 7 h and 8 h, respectively, which was not much different from that of the reference group of 7 h. It can be seen that the retardation effect is not good when these two super retarders are used individually at a dosage of 0.5%.
As can be seen in
Figure 2, after using 1.0% of super retarding agents, SDP-90, ACS and PBTCA three super retarding agents make the slurry recycled water setting time more than 14 h, it can be seen that these three super retarding agents 1.0% dosage retarding effect is better. Among them, PBTCA super retarding agent has the best effect on retardation of slurry recycling water, and the final measurement of the beginning of setting time is 18 h. However, when using AA/AMPS or PAPEMP these two super retarding agents, the setting time of waste slurry recycled water is 7.5 h and 9.5 h respectively, which is not much different from the reference group of 7 h; when using HEDP-4Na or IDS these two super retarding agents, the setting time of waste slurry recycled water is 10.5 h and 11 h respectively, which is insignificant compared to the reference group of retarding setting time. It can be seen that 1.0% dosage of AA/AMPS, PAPEMP retardation effect is not good, HEDP-4Na, IDS retardation effect is general.
As can be seen in
Figure 2, after using 1.5% of super retarding agents, the three super retarders SDP-90, ACS and PBTCA make the slurry recycled water setting time more than 18 h, which can be seen that these three super retarders are more effective in the dosage of 1.5% to slow down the sloughing effect. Among them, PBTCA super retarding agent has the best effect on retardation of slurry recycling water, and the final measured start of setting time is 22.5 h. However, when using HEDP-4Na or IDS, the setting time of waste slurry recycled water is 12 h, which is not obvious compared with the reference group; when using AA/AMPS or PAPEMP, the setting time of waste slurry recycled water is 8 h and 10 h, which is not much different from the reference group of 7 h; It can be seen that at 1.5% dosage of super retarding agent, the retarding effect of HEDP-4Na and IDS is general, and the retarding effect of AA/AMPS and PAPEMP is not good.
As can be seen in
Figure 2, after using 2.0% of super retarding agents, the two super retarders ACS and PBTCA made the slurry recycled water setting time more than 27 h, which can be seen that the two super retarders in the dosage of 2.0% retardation effect is better. Among them, PBTCA super retarding agent has the best effect on retarding the condensation of waste slurry recycled water, and the final measured time of the beginning of condensation is 30 h. However, when using the two super retarding agents HEDP-4Na or IDS, the setting time of waste slurry recycled water is 14 h and 17 h respectively, which is not obvious compared with the reference group; when using the two super retarding agents AA/AMPS or PAPEMP, the setting time of waste slurry recycled water is 9 h and 11 h respectively, which is not much different from the reference group of 7 h. It can be seen that 2.0% dosage of super retarding agent HEDP-4Na, IDS retarding effect in general, AA/AMPS, PAPEMP retarding effect is not good.
4.2. The Effect of Super Retarder on the Setting Time of Waste Slurry Recycling Water Under the Condition of Compound Mixing
ACS is a special super retarder for waste slurry water from concrete mixing plant which is currently used on a small scale, therefore, ACS was selected to be compounded with other super retarders with a view to obtaining a better retardation effect.
The six super retarding agents used under single blending conditions were compounded with ACS in the ratio of 1:20, and the compounded reagents were mixed with tap water in the ratio of 1:15 to make six super retarding solutions. According to the proportion of 1.5% of the total amount of recycled water (external mixing method) was added to different concentrations of waste pulp recycled water to determine the setting time of waste pulp recycled water.
Figure 3 shows the effects of different kinds of compounded super retarding agents on the setting time of waste slurry recycled water. The concentrations of the waste slurry recycled water were 7%, 10%, 15% and 20%.
As can be seen from
Figure 3, compared with single blending, the retardation effect of super retardant is significantly improved after compounding with ACS. When the concentration of slurry recycled water is 7%, PBTCA or SDP-90 compounded with ACS make the setting time of waste slurry recycled water more than 70 h. Among them, the setting time of waste slurry recycled water after compounding of PBTCA and ACS reaches 73 h, with a significant retardation effect. HEDP-4Na or IDS compounded with ACS made the setting time of waste slurry recycled water reach about 50 h, and the effect of retardation was general; AA/AMPS or PAPEMP compounded with ACS made the setting time of waste slurry recycled water reach about 40 h, and the effect of retardation was poor.
As can be seen from
Figure 3, when the concentration of slurry recycled water is 10%, PBTCA or SDP-90 compounded with ACS make the setting time of waste slurry recycled water more than 60 h. Among them, after the compounding of PBTCA and ACS, the setting time of waste slurry recycled water reached 64 h, and the effect of retardation was very significant; after the compounding of HEDP-4Na or IDS with ACS, the setting time of waste slurry recycled water reached about 40 h, and the effect of retardation was general; after the compounding of AA/AMPS or PAPEMP with ACS, the setting time of waste slurry recycled water reached about 60 h, and the effect of retardation was general; after the compounding of AA/AMPS or PAPEMP with ACS, the effect of retardation was very significant. After compounding AA/AMPS or PAPEMP with ACS, the setting time of waste slurry recycled water reached about 30 h, and the effect of retarding coagulation was poor.
As can be seen from
Figure 3, when the concentration of slurry recycled water is 15%, SDP-90 or PBTCA compounded with ACS make the waste slurry recycled water setting time are more than 45 h. Among them, ACS and PBTCA compounding, make the waste slurry recycled water setting time reached 49 h, the best effect of retardation. After the compounding of HEDP-4Na or IDS with ACS, the setting time of waste slurry recycled water reached about 40 h, and the effect of retarding coagulation was average; after the compounding of AA/AMPS or PAPEMP with ACS, the setting time of waste slurry recycled water reached about 30 h, and the effect of retarding coagulation was poor.
As can be seen from
Figure 3, when the concentration of slurry recycled water is 20%, The super retarders such as HEDP-4Na, PBTCA, etc., compounded with ACS have similar effects in delaying coagulation. Among them, PBTCA, IDS, SDP-90 compounded with ACS made the setting time of waste slurry recovery water reach about 35 h; HEDP-4Na, AA/AMPS, PAPEMP compounded with ACS made the setting time of waste slurry recovery water of reach about 30 h. It can be seen that when the concentration of waste slurry recycled water is higher, the compounding super retarder can delay the setting time to a certain extent, but the delaying effect is not obvious, and the delaying effect of each compounding super retarder is not much different.
4.3. Effect of Compounding Super Retarder on Concrete Properties
ACS+PBTCA and ACS+SDP-90, which have good retarding effect under compound mixing conditions, were selected, and the compounding ratios of the two groups of super retarding agents were changed respectively to study their effects on the working performance and compressive strength of concrete. The results of working performance test are shown in
Table 3 and
Table 4, and the results of compressive strength test are shown in
Figure 4 and
Figure 5.
As shown in
Table 3, compared to the reference group, the slump and extensibility of concrete exhibited a pattern of initial increase followed by decrease as the ratio of PBTCA to ACS increased. When PBTCA:ACS reached 1:20, there was no loss of 1 h slump and the loss of 1 h extensibility was 15 mm. Concrete has good workability in this condition.
Table 4 shows the effect of SDP-90 compounded with ACS at different ratios and added to waste slurry recycling water on the slump, extension, 1 h slump and 1 h extension of concrete at 1.5% admixture. As can be seen from
Table 4, with the increase of the ratio of PBTCA to ACS, the slump and extensibility of concrete showed a decreasing trend. When SDP-90:ACS was 1:20, the 1 h slump loss was the smallest, only 5 mm; at this time, the extension loss was 85 mm. Compared with the reference group, when using the compound super retarder of SDP-90 and ACS, the 1 h slump loss of concrete were all significantly reduced, but the 1 h extension loss were all larger.
As can be seen from
Figure 4, after mixing the compound super retarder of PBTCA and ACS, the waste slurry recycled water did not adversely affect the compressive strength of concrete in both low and high ratios, but improved the 7 days and 28 days compressive strengths. When PBTCA:ACS was 1:20, the 7 days compressive strength was increased by 3.5 MPa and the 28 days compressive strength was increased by 3.0 MPa; when PBTCA:ACS was 1:30, the 7 days compressive strength was increased by 2.2 MPa and the 28 days compressive strength was increased by 5.5 MPa. As can be seen from
Figure 5, after admixing the compounded super retarding agent of SDP-90 and ACS, the waste slurry recycled water has little effect on the compressive strength of concrete, but the overall trend is decreasing, and when SDP-90:ACS is 1:10 and 1:20, the phenomenon of water secretion occurs.
In summary, although either PBTCA or SDP-90 compounded with ACS can effectively retard the setting time of waste slurry recycled water, the effect of waste slurry recycled water on the working and mechanical properties of concrete is minimized when using the super retarding additive compounded with PBTCA and ACS, and it can increase the 7 days and 28 days compressive strengths of concrete when PBTCA:ACS is 1:20.
4.4. Microanalysis
The super retarder PBTCA and ACS were selected with a fixed ratio of 1:20, and XRD, DTG, TG and other microscopic tests were used to study their effects on the hydration of cement in waste slurry recycled water at different ages. The dosages were 0.5%, 1.5% and 2.0% (external mixing method), and the concentration of waste slurry recycled water was 10%.
Study of the types and amounts of hydration products at different ages using XRD:
Figure 6 shows the effect of different dosages of ACS+PBTCA on the type and amount of cement hydration products in 10% concentration of waste slurry recycled water as characterized by XRD.
As can be seen from
Figure 6, the types of crystalline phases in the hydration products did not change at all ages after doping with ACS+PBTCA. The calcium alumina peak intensities of blank and ACS+PBTCA doped specimens with different amounts of ACS+PBTCA were similar for the specimens with ages of 1 day, 3 days and 7 days, and the calcium hydroxide peak intensities of ACS+PBTCA doped specimens with ages of 1 day and 3 days were lower than those of the blank specimens; The calcium hydroxide peak intensity of the 0.5% ACS+PBTCA doped specimen at the age of 7 days is higher than that of the blank specimen, and the calcium hydroxide peak intensity of the remaining two doped ACS+PBTCA specimens is similar, and both are lower than that of the blank group and the 0.5% ACS+PBTCA doped specimen group.
After adding ACS and PBTCA compound super retarder, it reacts with Ca(OH)2 on the surface of the generated clinker phase to form “insoluble” calcium phosphate, which hinders normal hydration and slows down the setting time of waste slurry recycled water. At the same time, after adding the compound super retarder, the content of C3S is obviously increased, so it is favorable to the compressive strength.
Study on the types and amounts of hydration products at different ages using DTG:
Four components were selected for the test, one group was a blank group and the remaining three groups were control groups with ACS+PBTCA. The concentration of recycled water was 10%. Thermogravimetric tests were performed on the four cement pastes separately. The changes in hydration products of the four pastes were analyzed at different hydration times.
Figure 7 shows the effect of different dosages of ACS+PBTCA on cement paste in recycled water as characterized by DTG.
As shown in
Figure 7, ACS+PBTCA does not cause new hydration products to appear in the cement paste. The more obvious characteristic peaks in the figure are the dehydration and heat absorption peak of free water or water of crystallization inside the decomposition of calcite near 100 °C, the CH decomposition peak near 430 °C and the CaCO
3 decomposition peak near 700 °C, in which CaCO
3 mainly comes from the raw materials in the cement, and a small amount of carbonation will occur in the cement during the storage process.
It can be seen that, with the advance of hydration time, the DTG curves of cement slurry and blank cement slurry in recycled water with 10% concentration of waste slurry doped with different amounts of ACS+PBTCA gradually converge, indicating that doping of ACS+PBTCA affects the rate of generation of hydration products, but does not have an effect on the type of cement hydration products.
Study of the types and amounts of hydration products at different ages using TG:
Figure 8 shows the effect of different dosages of ACS+PBTCA on cement paste in 10% concentration of waste slurry recycled water as characterized by TG.
As can be seen from
Figure 8, the hydration product has three distinct absorption peaks in the range of 45~900 °C, which are TG1: 45~400 °C, TG2: 400~540 °C, and TG3: 540~900 °C.
The combined water and CH volumes were calculated by the following equations, respectively:
where P1 is the percentage of bound water in CSH gel and AFt, P2 is the percentage of calcium hydroxide, P3 is the percentage of total bound water, and TG1 to TG3 are the three significant heat losses in the TG curve. The results of the analysis are shown in
Table 5.
As can be seen from
Table 5, the total bound water quantity of the blank and 0.5% ACS+PBTCA doped specimens gradually increased with the extension of age, the total bound water quantity of the 1.5% ACS+PBTCA doped specimens firstly increased and then decreased, and the total bound water quantity of the 2.0% ACS+PBTCA doped specimens firstly decreased and then increased. At early age (1~3 days), the CH and total bound water of ACS+PBTCA specimens doped with different dosages were lower than those of blank specimens. At the age of 7 days, the CH of the 0.5% ACS+PBTCA doped samples was higher than that of the blank samples, and the CH of the rest of the doped samples was lower than that of the blank samples.