AU2021101173A4 - Alkaline cementitious material of c-a-s-h seed crystal, preparation method and use thereof - Google Patents
Alkaline cementitious material of c-a-s-h seed crystal, preparation method and use thereof Download PDFInfo
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- AU2021101173A4 AU2021101173A4 AU2021101173A AU2021101173A AU2021101173A4 AU 2021101173 A4 AU2021101173 A4 AU 2021101173A4 AU 2021101173 A AU2021101173 A AU 2021101173A AU 2021101173 A AU2021101173 A AU 2021101173A AU 2021101173 A4 AU2021101173 A4 AU 2021101173A4
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- seed crystal
- cementitious material
- nano
- alkaline cementitious
- alkaline
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- 239000000463 material Substances 0.000 title claims abstract description 55
- 239000013078 crystal Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 239000011398 Portland cement Substances 0.000 claims abstract description 11
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 9
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 9
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 9
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims abstract description 9
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 8
- 239000011575 calcium Substances 0.000 claims description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- 239000004568 cement Substances 0.000 abstract description 38
- 239000000243 solution Substances 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 3
- 239000000499 gel Substances 0.000 abstract description 3
- 239000004576 sand Substances 0.000 description 8
- JLDKGEDPBONMDR-UHFFFAOYSA-N calcium;dioxido(oxo)silane;hydrate Chemical compound O.[Ca+2].[O-][Si]([O-])=O JLDKGEDPBONMDR-UHFFFAOYSA-N 0.000 description 4
- 239000011083 cement mortar Substances 0.000 description 4
- 238000007580 dry-mixing Methods 0.000 description 3
- 230000036571 hydration Effects 0.000 description 3
- 238000006703 hydration reaction Methods 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- -1 polytetrafluoroethylene Polymers 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000000378 calcium silicate Substances 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
- C04B22/0086—Seeding materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/04—Portland cements
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/20—Retarders
- C04B2103/22—Set retarders
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The present disclosure relates to an alkaline cementitious material of C-A-S-H seed crystals, a
preparation method and a use thereof. The preparation method thereof comprises: Calcium
hydroxide, nano-silica, nano-alumina and deionized water are weighed; nano-silica and nano
alumina are mixed with deionized water, and ultrasonically dispersed to obtain a mixed
solution; calcium hydroxide is then added to the mixed solution, and ultrasonically dispersed to
obtain a mixed material; the mixed material is sealed in a reaction vessel, and the reaction vessel
is heated and stirred on a stirrer; the reaction vessel is placed in a water bath and cured to an age
of 3 to 7 days; the cured product is washed and filtered with absolute ethanol and deionized
water, which is repeated twice or more; the product is dried in a vacuum environment to obtain
an alkaline cementitious material of C-A-S-H seed crystal. And the above alkaline cementitious
material of C-A-S-H seed crystal is used for improving the mechanical strength of a Portland
cement system. The above technical solutions can effectively address the poor moisture
resistance, heat resistance, and corrosion resistance of existing cement caused by the addition of
C-S-H gels as well as the reduced service life and limited scope of application thereof.
1/2
DRAWINGS:
25000- C
20000- -C-A-S-H
15000
10000- C
5000- C
0
0 10 20 30 40 50 60 70 80
20
FIG. 1
FIG. 2
Description
1/2
25000- C
20000- -C-A-S-H
15000
10000- C
5000- C
0
0 10 20 30 40 50 60 70 80 20
FIG. 1
FIG. 2
[0001] The present disclosure relates to the technical field of C-A-S-H seed crystals, in particular to an alkaline cementitious material of C-A-S-H seed crystal, a preparation method thereof and a use for improving the early strength of Portland cement.
[0002] Due to social development, there is a higher demand on the performance of cement materials. On one hand, common Portland cement is required to have improved compressive strength and flexural strength. On the other hand, cement needs to have specific properties to meet special purposes under special circumstances. Calcium silicate hydrate (C-S-H) is the main hydration product of cementitious materials, accounting for 60-70 wt% thereof, which serves as the most important source of strength for cementitious materials. In order to improve the performance of cementitious materials, artificially synthesized C-S-H gels are added to cementitious materials, which improves the performance; however, due to the defects in the structure of C-S-H itself, the moisture resistance, heat resistance, and corrosion resistance are poor, which affects its applicable properties, reduces its service life, and limits its scope of application. Therefore, it is urgent to design a new technical solution to comprehensively solve the problems existing in the prior art.
[0003] It is an object of the present disclosure to provide an alkaline cementitious material of C A-S-H seed crystal and a preparation method thereof, which can effectively address the poor moisture resistance, heat resistance, and corrosion resistance of existing cement caused by the addition of C-S-H gels as well as the reduced service life and limited scope of application thereof.
[0004] To solve the above technical problems, the present disclosure adopts the following technical solutions:
[0005] A method for the preparation of an alkaline cementitious material of C-A-S-H seed crystal is provided, which comprises the following steps:
[0006] Step S1. Calcium hydroxide, nano-silica, nano-alumina and deionized water are weighed according to a Ca/Si ratio of 1.0 to 2.0, a Si/Al ratio of 2.0 to 3.0, and a water/solid ratio of 6.0 to 9.0; nano-silica and nano-alumina are mixed with deionized water, and ultrasonically dispersed to obtain a mixed solution; calcium hydroxide is then added to the mixed solution, and ultrasonically dispersed to obtain a mixed material;
[0007] Step S2. The mixed material obtained in step S Iis sealed in a reaction vessel, and the reaction vessel is heated and stirred on a thermostatic magnetic stirrer at 60°C for 60 to 90 minutes;
[0008] Step S3. The reaction vessel of step S2 is placed in a water bath at 25 to 95°C and cured to an age of 3 to 7 days;
[0009] Step S4. The cured product in step S3 is washed and filtered with absolute ethanol and deionized water, which is repeated twice or more;
[0010] Step S5. The product obtained in step S4 is dried in a vacuum environment to a constant weight to obtain an alkaline cementitious material of C-A-S-H seed crystal.
[0011] The time of ultrasonic dispersion in step S is 3 minutes; the sealing process in step S2 is performed in a N 2 atmosphere; the drying temperature of the vacuum environment in step S5 is 55 to 65°C.
[0012] A use of an alkaline cementitious material of C-A-S-H seed crystal for improving the mechanical strength of a Portland cement system is also provided, wherein the addition amount of the alkaline cementitious material of C-A-S-H seed crystal is 1% to 5% by mass of the Portland cement material.
[0013] The method for the preparation of an alkaline cementitious material of C-A-S-H seed crystal, the alkaline cementitious material of C-A-S-H seed crystal prepared by the method, and the use of the alkaline cementitious material of C-A-S-H seed crystal for improving the mechanical strength of a Portland cement system as provided in the above technical solutions can effectively promote the hydration of cement and shorten the setting time of cement. Meanwhile, the present disclosure is suitable for construction projects of cement systems, can refine the pore structure, reduce the porosity of hardened paste, and improve the early strength of Portland cement, which is beneficial to the low carbonization and green development of cement, and has good environmental protection benefits as well as social and economic benefits. In addition, the present disclosure prepares an alkaline cementitious material of C-A-S H seed crystal by hydrothermal method using nano-silica, nano-alumina and calcium hydroxide, which is excellent in avoiding carbonization. The preparation process is simple; the product performance is stable; and the product has a good application prospect.
[0014] FIG. 1 is an XRD pattern of an alkaline cementitious material of C-A-S-H seed crystal prepared in the example;
[0015] FIG. 2 is an SEM chart of an alkaline cementitious material of C-A-S-H seed crystal prepared in the example;
[0016] FIG. 3 is a comparison diagram showing the flexural strength of mortar test blocks with different addition amounts of an alkaline cementitious material of C-A-S-H seed crystal at different ages;
[0017] FIG. 4 is a comparison diagram showing the compressive strength of mortar test blocks with different addition amounts of an alkaline cementitious material of C-A-S-H seed crystal at different ages.
[0018] In order to make the objects and advantages of the present disclosure clearer, the present disclosure is described hereinbelow in conjunction with examples. It should be understood that the following is only used to describe one or more specific embodiments of the present disclosure, and does not strictly limit the protection scope that is specifically asked for in the present disclosure.
[0019] An alkaline cementitious material of C-A-S-H seed crystal was first prepared:
[0020] Step S. 32 g of calcium hydroxide, 25.9 g of nano-silica, 22.1 g of nano-alumina and 640 g of deionized water were weighed according to a Ca/Si ratio (a ratio of calcium to silicon) of 1.0, a Si/Al ratio (a ratio of silicon to aluminum) of 2.0, and a water/solid ratio (a ratio of deionized water to the sum of the calcareous material, aluminum material and siliceous material) of 8; nano-silica and nano-alumina were mixed with deionized water, and ultrasonically dispersed for 3 minutes to obtain a mixed solution; calcium hydroxide was then added to the mixed solution, and ultrasonically dispersed for 3 minutes to obtain a mixed material;
[0021] Step S2. The mixed material obtained in step S was sealed in a polytetrafluoroethylene reaction vessel in a N 2 atmosphere, and the polytetrafluoroethylene reaction vessel was heated and stirred on a thermostatic magnetic stirrer at 60°C for 90 minutes;
[0022] Step S3. The polytetrafluoroethylene reaction vessel of step S2 was placed in a water bath at 60°C and cured to an age of 3 days;
[0023] Step S4. The cured product in step S3 was washed and filtered with absolute ethanol and deionized water, which was repeated twice;
[0024] Step S5. The product obtained in step S4 was dried at 60°C in a vacuum environment to a constant weight to obtain an alkaline cementitious material of C-A-S-H seed crystal.
[0025] Example 1
[0026] A cement paste was prepared at a water to cement ratio of 0.34 without adding an alkaline cementitious material of C-A-S-H seed crystal, and the setting time was tested. The results of setting time are shown in Table 1. And a cement mortar was prepared at a water to cement ratio of 0.54, and a mass ratio of cement to standard sand (cement to sand ratio) of 1 : 3 without adding an alkaline cementitious material of C-A-S-H seed crystal, which was molded and cured. The strength at different ages was measured, and the results strength tests are shown in FIG. 3 and FIG. 4.
[0027] Example 2
[0028] A cement paste was prepared at a water to cement ratio of 0.34; an alkaline cementitious material of C-A-S-H seed crystal was added in an amount of 1% (by mass of the cement), and subjected to a graded dry mixing with the cement. The setting time was tested, and the results of setting time are shown in Table 1. And a cement mortar was prepared at a water to cement ratio of 0.54, and a mass ratio of cement to standard sand (cement to sand ratio) of 1 : 3; an alkaline cementitious material of C-A-S-H seed crystal was added in an amount of 1% (by mass of the cement), molded and cured. The strength at different ages was measured, and the results of strength tests are shown in FIG. 3 and FIG. 4.
[0029] Example 3
[0030] A cement paste was prepared at a water to cement ratio of 0.34; an alkaline cementitious material of C-A-S-H seed crystal was added in an amount of 3% (by mass of the cement), and subjected to a graded dry mixing with the cement. The setting time was tested, and the results of setting time are shown in Table 1. And a cement mortar was prepared at a water to cement ratio of 0.54, and a mass ratio of cement to standard sand (cement to sand ratio) of 1 : 3; an alkaline cementitious material of C-A-S-H seed crystal was added in an amount of 3% (by mass of the cement), molded and cured. The strength at different ages was measured, and the results of strength tests are shown in FIG. 3 and FIG. 4.
[0031] Example 4
[0032] A cement paste was prepared at a water to cement ratio of 0.34; an alkaline cementitious material of C-A-S-H seed crystal was added in an amount of 5% (by mass of the cement), and subjected to a graded dry mixing with the cement. The setting time was tested, and the results of setting time are shown in Table 1. And a cement mortar was prepared at a water to cement ratio of 0.54, and a mass ratio of cement to standard sand (cement to sand ratio) of 1 : 3; an alkaline cementitious material of C-A-S-H seed crystal was added in an amount of 5% (by mass of the cement), molded and cured. The strength at different ages was measured, and the results of strength tests are shown in FIG. 3 and FIG. 4.
[0033] Table 1 Comparison of cement paste setting time with different addition amounts of C A-S-H Example 1 Example 2 Example 3 Example 4 Water consumption for 34 34 34 34 standard consistency/% Initial setting time/min 176 132 112 74 Final setting time/min 274 212 145 114
[0034] It can be seen from Table 1, FIG. 3 and FIG. 4 that the addition of C-A-S-H seed crystals can promote the hydration of Portland cement and significantly reduce the setting time. The higher the addition amount, the shorter the setting time. However, the strength of the mortar was not directly proportional to the addition amount of C-A-S-H seed crystals. When the addition amount was 1%, the strength improvement effect was the best. As the amount increased, the strength did not increase but decreased.
[0035] The embodiments of the present disclosure are described hereinabove in conjunction with the examples, but the present disclosure is not limited to the above embodiments. For those of ordinary skill in the art, after learning the contents of the present disclosure, they may also make equivalent variations and substitutions without departing from the principle of the present disclosure. These equivalent variations and substitutions should also be regarded within the protection scope of the present disclosure.
Claims (5)
1. A method for the preparation of an alkaline cementitious material of C-A-S-H seed crystal, wherein the method comprises the following steps: Step S1. Calcium hydroxide, nano-silica, nano-alumina and deionized water are weighed according to a Ca/Si ratio of 1.0 to 2.0, a Si/Al ratio of 2.0 to 3.0, and a water/solid ratio of 6.0 to 9.0; nano-silica and nano-alumina are mixed with deionized water, and ultrasonically dispersed to obtain a mixed solution; calcium hydroxide is then added to the mixed solution, and ultrasonically dispersed to obtain a mixed material; Step S2. The mixed material obtained in step S Iis sealed in a reaction vessel, and the reaction vessel is heated and stirred on a thermostatic magnetic stirrer at 60°C for 60 to 90 minutes; Step S3. The reaction vessel of step S2 is placed in a water bath at 25 to 95°C and cured to an age of 3 to 7 days; Step S4. The cured product in step S3 is washed and filtered with absolute ethanol and deionized water, which is repeated twice or more; Step S5. The product obtained in step S4 is dried in a vacuum environment to a constant weight to obtain an alkaline cementitious material of C-A-S-H seed crystal; wherein the time of ultrasonic dispersion in step S is 3 minutes; the sealing process in step S2 is performed in a N 2 atmosphere; the drying temperature of the vacuum environment in step S5 is 55 to 65°C.
2. An alkaline cementitious material of C-A-S-H seed crystal, wherein it is prepared by the method for the preparation of an alkaline cementitious material of C-A-S-H seed crystal according to claim 1.
3. A use of an alkaline cementitious material of C-A-S-H seed crystal for improving the mechanical strength of a Portland cement system.
4. The use according to claim 3, wherein the addition amount of the alkaline cementitious material of C-A-S-H seed crystal is 1% to 5% by mass of the Portland cement material.
5. The use according to claim 4, wherein the addition amount of the alkaline cementitious material of C-A-S-H seed crystal is 1% by mass of the Portland cement material.
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CN114956721A (en) * | 2022-05-06 | 2022-08-30 | 山西中科赛德能源科技有限公司 | High-strength superfine deep hole grouting reinforcement material and preparation method thereof |
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CN114956721A (en) * | 2022-05-06 | 2022-08-30 | 山西中科赛德能源科技有限公司 | High-strength superfine deep hole grouting reinforcement material and preparation method thereof |
CN114956721B (en) * | 2022-05-06 | 2023-05-23 | 山西中科赛德能源科技有限公司 | High-strength superfine deep hole grouting reinforcement material and preparation method thereof |
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