CN108083758B - Magnesium oxysulfate cement-based composite material and preparation method thereof - Google Patents
Magnesium oxysulfate cement-based composite material and preparation method thereof Download PDFInfo
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- CN108083758B CN108083758B CN201810051669.1A CN201810051669A CN108083758B CN 108083758 B CN108083758 B CN 108083758B CN 201810051669 A CN201810051669 A CN 201810051669A CN 108083758 B CN108083758 B CN 108083758B
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- 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
- C04B28/30—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 magnesium cements or similar cements
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Abstract
The invention discloses a magnesium oxysulfate cement-based composite material and a preparation method thereof, wherein the composite material comprises graphene, a nano material dispersing agent, a defoaming agent, micro silica gel powder, starch, a magnesium sulfate solution and light-burned MgO powder; the preparation method comprises the steps of uniformly mixing graphene, a nano material dispersing agent, micro silica gel powder and starch, adding the mixture into a magnesium sulfate solution, dispersing to obtain a mixed solution, then mixing and uniformly stirring the mixed solution, a defoaming agent and light-burned MgO powder, pouring the mixture into a mold, molding for 12-36 hours, demolding, and maintaining. The magnesium oxysulfate cement-based composite material has the remarkable advantages that the magnesium oxysulfate cement-based composite material has high tensile strength, and compared with the traditional magnesium oxysulfate cement material without graphene, the magnesium oxysulfate cement-based composite material has the advantages that the tensile strength is improved by 68-144.9%, and the magnesium oxysulfate cement-based composite material has excellent durability and reliability; meanwhile, the preparation method is simple, the process is easy to control, the cost is low, and the energy is saved and the environment is protected.
Description
Technical Field
The invention belongs to the field of cement materials, and particularly relates to a magnesium oxysulfate cement-based composite material and a preparation method thereof.
Background
The magnesium oxysulfate cement is prepared from active MgO and MgSO with a certain concentration4MgO-MgSO formed by solution preparation4-H2The O ternary cementing system has the characteristics of quick setting and hardening, high early strength, good cohesiveness, no need of wet maintenance, low thermal conductivity, high fire resistance, good wear resistance, excellent corrosion resistance and the like, has low production energy consumption and simple preparation process, and can be widely applied to the production of light heat-insulating wallboards, refractory materials, decorative and finishing materials for buildings, oil well leakage stoppage and other projects. However, the magnesium oxysulfate cement before modification has low tensile strength, is easy to have uneven stress in practical application, causes the reduction of structural durability, and seriously limits the application. With the intensive research on the magnesium oxysulfate cement, the magnesium oxysulfate cement is doped with citric acid to generate a new 5Mg (OH)2·MgSO4·7H2And the O crystal phase (517 phase) has improved physical and mechanical properties. The filling effect of the fly ash particles can enable the magnesium oxysulfate cement paste to be more compact, so that the compressive strength of the cement paste is improved. However, the research on improving the flexural strength of magnesium oxysulfate cement is not extensive.
The graphene is a honeycomb lattice structure consisting of carbon six-membered rings, and has excellent mechanical, electrical and optical properties due to the unique two-dimensional lattice structure. Therefore, the composite material can be used as an ideal reinforcing material, endows the composite material with more excellent performance, and expands the application field of the composite material. The graphene has excellent mechanical properties, good flexibility and huge specific surface area, so that the graphene and the magnesium oxysulfate cement are well compounded, the complementary advantages or the reinforcement of the two materials can be realized, the tensile strength of the magnesium oxysulfate cement-based material can be greatly improved, the durability and the reliability are improved, the novel performance is endowed, and the graphene has strong development power in engineering materials. However, the graphene has low surface energy and weak interface action with cement, so that the dispersion effect is poor. Therefore, a magnesium oxysulfate cement composite material with high tensile strength is needed to be prepared by effectively improving the dispersion effect of graphene in cement.
Disclosure of Invention
The purpose of the invention is as follows: the first purpose of the invention is to provide a magnesium oxysulfate cement-based composite material with high tensile strength; the second purpose of the invention is to provide a preparation method of the composite material.
The technical scheme is as follows: the magnesium oxysulfate cement-based composite material comprises the following raw materials: graphene, a nano-material dispersing agent, a defoaming agent, micro-powder silica gel, starch, a magnesium sulfate solution and light-burned MgO powder; wherein the graphene accounts for 0.02-2.0% of the weight of the light-burned MgO powder, and the mass ratio of the graphene, the nano material dispersing agent, the defoaming agent, the micro silica gel powder and the starch is 1 (0.005-0.05), (0.002-0.01), (0.003-0.03) and (0.02-0.3).
According to the invention, the micro silica gel powder, the starch and the nano material dispersing agent are added into the raw materials, so that the micro silica gel powder, the starch and the nano material dispersing agent act synergistically, the uniform dispersing force of the graphene in the cement is improved, the graphene is completely doped into the magnesium oxysulfate cement, and the acting force with a cement interface is improved. Preferably, the mass ratio of the graphene to the nano-material dispersant to the defoamer to the silica gel micropowder to the starch can be 1 (0.01-0.03): (0.005-0.008): 0.007-0.01): 0.06-0.2), and the graphene, the nano-material dispersant, the silica gel micropowder and the starch can be better dissolved in the content range, so that the dispersibility of the graphene in the cement is improved.
Furthermore, the thickness of the graphene adopted by the invention is 2.0-4.0 nm, and the specific surface area is 360-450 m2The thickness range and the specific surface area range can enable the graphene to be better dispersed in the cement.
Still further, the defoaming agent may include tributyl phosphate or dimethicone. The nanomaterial dispersant may include sodium dodecylbenzenesulfonate, sodium cholate or polyvinylpyrrolidone. The mass percentage concentration of the magnesium sulfate solution can be 0.28-0.33. The molar ratio of the light-burned MgO powder to the magnesium sulfate can be 7-9: 1.
The method for preparing the magnesium oxysulfate cement-based composite material comprises the following steps of:
(1) uniformly mixing graphene, a nano material dispersant, micro silica gel powder and starch, adding into a magnesium sulfate solution, and dispersing to obtain a mixed solution;
(2) and mixing and uniformly stirring the mixed solution, the defoaming agent and the light-burned MgO powder, pouring the mixture into a mold for molding for 12-36 h, demolding and maintaining.
Furthermore, the curing is carried out under the conditions that the relative humidity is 57-70% and the temperature is 19-25 ℃. Under the maintenance condition, the hydration of the module is sufficient, and the influence of overlarge or overhigh relative humidity on the strength is large.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages: the magnesium oxysulfate cement-based composite material has high tensile strength, and compared with the traditional magnesium oxysulfate cement material without graphene, the tensile strength is improved by 68-144.9%, and the magnesium oxysulfate cement-based composite material has excellent durability and reliability; meanwhile, the preparation method is simple, the process is easy to control, the cost is low, and the energy is saved and the environment is protected.
Drawings
FIG. 1 is a microscopic topography of graphene employed in the present invention;
FIG. 2 is a microscopic morphology of the magnesium oxysulfate cement hardened slurry with 0.02% graphene doping amount according to the present invention;
FIG. 3 is a microscopic morphology of the magnesium oxysulfate cement hardened slurry with 0.5% graphene doping amount according to the present invention;
FIG. 4 is a microscopic morphology of the magnesium oxysulfate cement hardened slurry with a graphene doping amount of 1.0% according to the present invention.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to the accompanying drawings and embodiments.
The raw materials adopted by the invention can be purchased from the market, the thickness of the adopted graphene is 2.0-4.0 nm, and the specific surface area is 360-450 m2/g。
Example 1
Raw materials: graphene, sodium dodecyl benzene sulfonate, tributyl phosphate, micro powder silica gel, starch, magnesium sulfate solution and light-burned MgO powder; the weight ratio of the graphene, the sodium dodecyl benzene sulfonate, the tributyl phosphate, the micro powder silica gel and the starch is 1:0.02:0.007:0.009:0.1, the graphene accounts for 0.02% of the weight of the light-burned MgO powder, and the molar ratio of the light-burned MgO powder to the magnesium sulfate is 7: 1.
The preparation method comprises the following steps:
(1) weighing distilled water and magnesium sulfate heptahydrate, and preparing a magnesium sulfate solution with the mass concentration of 0.3;
(2) uniformly mixing graphene, sodium dodecyl benzene sulfonate, micro powder silica gel and starch, adding into the magnesium sulfate solution, and dispersing for 40min to obtain a mixed solution;
(3) and mixing and uniformly stirring the mixed solution, tributyl phosphate and light-burned MgO powder, pouring the mixture into a mold for molding for 25 hours, demolding, and curing for 28 days at the relative humidity of 60% and the temperature of 22 ℃ to obtain the magnesium oxysulfate cement-based composite material.
Example 2
Raw materials: graphene, sodium dodecyl benzene sulfonate, tributyl phosphate, micro powder silica gel, starch, magnesium sulfate solution and light-burned MgO powder; the weight ratio of the graphene to the sodium dodecyl benzene sulfonate to the tributyl phosphate to the silica gel micropowder to the starch is 1:0.01:0.008:0.007:0.2, the graphene accounts for 0.5% of the weight of the light-burned MgO powder, and the molar ratio of the light-burned MgO powder to the magnesium sulfate is 8: 1.
The preparation method comprises the following steps:
(1) weighing distilled water and magnesium sulfate heptahydrate, and preparing a magnesium sulfate solution with the mass concentration of 0.33;
(2) uniformly mixing graphene, sodium dodecyl benzene sulfonate, micro powder silica gel and starch, adding into the magnesium sulfate solution, and dispersing for 40min to obtain a mixed solution;
(3) and mixing and uniformly stirring the mixed solution, tributyl phosphate and light-burned MgO powder, pouring the mixture into a mold for molding for 12 hours, demolding, and curing for 28 days under the conditions that the relative humidity is 70% and the temperature is 19 ℃ to obtain the magnesium oxysulfate cement-based composite material.
Example 3
Raw materials: graphene, sodium dodecyl benzene sulfonate, tributyl phosphate, micro powder silica gel, starch, magnesium sulfate solution and light-burned MgO powder; the weight ratio of the graphene to the sodium dodecyl benzene sulfonate to the tributyl phosphate to the silica gel micropowder to the starch is 1:0.03:0.005:0.01:0.06, the graphene accounts for 1% of the weight of the light-burned MgO powder, and the molar ratio of the light-burned MgO powder to the magnesium sulfate is 8: 1.
The preparation method comprises the following steps:
(1) weighing distilled water and magnesium sulfate heptahydrate, and preparing a magnesium sulfate solution with the mass concentration of 0.28;
(2) uniformly mixing graphene, sodium dodecyl benzene sulfonate, micro powder silica gel and starch, adding into the magnesium sulfate solution, and dispersing for 40min to obtain a mixed solution;
(3) and mixing the mixed solution, the dimethyl silicone oil and the light-burned MgO powder, uniformly stirring, pouring into a mould for forming for 36 hours, demoulding, and curing for 28 days at the relative humidity of 57% and the temperature of 25 ℃ to obtain the magnesium oxysulfate cement-based composite material.
The magnesium oxysulfate cement-based composite materials prepared in examples 1 to 3 were subjected to mechanical property tests according to a standard mechanical property test method (refer to standard GBT50081-2002), and compared with a conventional magnesium oxysulfate cement test piece to which graphene was not added, and the results obtained are shown in table 1 below and fig. 1 to 4.
TABLE 1 tensile Properties of composites prepared in examples 1-3
As can be seen from table 1, the tensile strength of the magnesium oxysulfate cement-based composite material prepared by the method is respectively increased by 70%, 95.8% and 121.2% compared with that of the conventional magnesium oxysulfate cement test piece without adding graphene, and thus, the magnesium oxysulfate cement-based composite material has high tensile strength. Meanwhile, as can be seen from fig. 1 to 4, the graphene can be doped into the magnesium oxysulfate cement, the large specific surface area enables the graphene to play a good filling and bridging role in a magnesium oxysulfate cement matrix, the good flexibility of the graphene enables the graphene to be capable of remarkably improving the tensile strength and the fracture resistance of the magnesium oxysulfate cement, and the higher the graphene doping amount is within the range of 0.02 to 2.0%, the more obvious the enhancement effect is.
Example 4
6 sets of parallel tests are designed, the basic steps are the same as those in example 1, except that the content of graphene respectively accounts for 0.01%, 0.02%, 0.08%, 1.5%, 2% and 2.1% of the weight of the light-burned MgO powder, and the tensile property of the prepared magnesium oxysulfate cement-based composite material is detected, and the obtained results are shown in the following table 2.
Table 2 tensile properties of the composite material prepared in example 4
As can be seen from Table 2, the magnesium oxysulfate cement-based composite material prepared by adding graphene accounting for 0.02-2.0% of the weight of the light-burned MgO powder has strong tensile property, because the graphene is doped into the magnesium oxysulfate cement, the clustered graphene particles are uniformly dispersed in the matrix, hydration products are refined and distributed more uniformly, the large specific surface area enables the composite material to play a good role in filling and bridging in the magnesium oxysulfate cement matrix, and meanwhile, the good flexibility of the graphene enables the composite material to remarkably improve the tensile property and the folding resistance of the magnesium oxysulfate cement. If the content of graphene is less, the distance between graphene particles is larger, the intermolecular force is weaker, and the influence on the strength is not obvious.
Example 5
Design 5 sets of parallel tests, the basic steps are the same as those of example 1, except that the mass ratio of graphene, nanomaterial dispersant, defoamer, silica gel micropowder and starch is (1:0.004:0.02:0.002:0.4), (1:0.005:0.01:0.003:0.3), (1:0.02:0.007:0.009:0.1), (1:0.05:0.002:0.03:0.02), (1:0.006:0.001:0.04:0.01), and the prepared magnesium oxysulfate cement-based composite material is subjected to tensile property detection, and the obtained results are shown in table 3 below.
Table 3 tensile properties of the composite material prepared in example 5
As can be seen from table 3, the magnesium oxysulfate cement-based composite material prepared by using the mass ratio of graphene, nanomaterial dispersant, defoamer, silica gel micropowder and starch in the range of (0.005-0.05): (0.002-0.01): 0.003-0.03): 0.02-0.3 has strong tensile strength, while the mass ratio of graphene, nanomaterial dispersant, defoamer, silica gel micropowder and starch exceeds the range of the present invention, such as the mass ratio of the groups 1 and 5, the composite material prepared by using the method has poor tensile strength, because large-scale clustering occurs among graphene particles when the graphene doping amount is relatively large, and the graphene volume is relatively large, and the original integrity of a hydrated matrix is destroyed when the clustering volume is relatively large; when the graphene is mixed in a large amount, a large water-cement ratio is required for ensuring the workability of cement paste, and when the water-cement ratio is large, the light-burned magnesia absorbs more water to generate expansive Mg (OH)2Thereby increasing the internal pores of the set cement and further hindering the development of strength.
Comparative example 1
The basic procedure was the same as in example 1, except that no aerosil was added to the raw materials, and the composite material prepared in this comparative example was subjected to performance testing, and the results obtained are shown in table 4.
TABLE 4 comparison of Properties of composite materials prepared in comparative example 1 and example 1
Comparative example 2
The basic procedure was the same as in example 1, except that no starch was added to the raw materials, and the composite material prepared in this comparative example was subjected to the performance test, and the results obtained are shown in table 5.
TABLE 5 comparison of Properties of composite materials prepared in comparative example 2 and example 1
It can be seen from tables 4 and 5 that the tensile strength of the material prepared without adding silica gel micropowder or starch in the raw material is weak, because the silica gel micropowder and the starch are added, the silica gel micropowder and the starch can act synergistically with the nanomaterial dispersant to improve the uniform dispersion force of graphene in cement, so that the graphene is completely doped into magnesium oxysulfate cement, and the acting force of the interface with the cement is improved, thereby fully playing the role of the graphene, improving the tensile strength of the magnesium oxysulfate cement-based composite material, and improving the tensile strength by 68-144.9% compared with the traditional magnesium oxysulfate cement material without adding graphene.
Example 6
The basic procedure is the same as example 1, except that the nanomaterial dispersant is sodium cholate or polyvinylpyrrolidone, and the molar ratio of MgO powder to magnesium sulfate is 9: 1.
Claims (9)
1. The magnesium oxysulfate cement-based composite material is characterized by comprising the following raw materials: graphene, a nano-material dispersing agent, a defoaming agent, micro-powder silica gel, starch, a magnesium sulfate solution and light-burned MgO powder; wherein the graphene accounts for 0.02-2.0% of the weight of the light-burned MgO powder, and the mass ratio of the graphene, the nano material dispersing agent, the defoaming agent, the micro silica gel powder and the starch is 1 (0.005-0.05), (0.002-0.01), (0.003-0.03) and (0.02-0.3).
2. The magnesium oxysulfate cement-based composite material according to claim 1, characterized in that: the mass ratio of the graphene, the nano-material dispersant, the defoaming agent, the micro-powder silica gel and the starch is 1 (0.01-0.03): (0.005-0.008): 0.007-0.01): 0.06-0.2.
3. The magnesium oxysulfate cement-based composite material according to claim 1, characterized in that: the thickness of the graphene is 2.0-4.0 nm, and the specific surface area is 360-450 m2/g。
4. The magnesium oxysulfate cement-based composite material according to claim 1, characterized in that: the nano material dispersant comprises sodium dodecyl benzene sulfonate, sodium cholate or polyvinylpyrrolidone.
5. The magnesium oxysulfate cement-based composite material according to claim 1, characterized in that: the defoaming agent comprises tributyl phosphate or dimethyl silicone oil.
6. The magnesium oxysulfate cement-based composite material according to claim 1, characterized in that: the mass concentration of the magnesium sulfate solution is 0.28-0.33.
7. The magnesium oxysulfate cement-based composite material according to claim 1, characterized in that: the molar ratio of the light-burned MgO powder to the magnesium sulfate is 7-9: 1.
8. A method of making the magnesium oxysulfate cement-based composite material of claim 1, comprising the steps of:
(1) uniformly mixing graphene, a nano material dispersant, micro silica gel powder and starch, adding into a magnesium sulfate solution, and dispersing to obtain a mixed solution;
(2) and mixing and uniformly stirring the mixed solution, the defoaming agent and the light-burned MgO powder, pouring the mixture into a mold for molding for 12-36 h, demolding and maintaining.
9. The method of preparing a magnesium oxysulfate cement-based composite material according to claim 8, characterized in that: in the step (2), the maintenance is carried out under the conditions that the relative humidity is 57-70% and the temperature is 19-25 ℃.
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| CN111471442B (en) * | 2020-04-30 | 2022-09-09 | 中国石油天然气集团有限公司 | Old well blasthole plugging and cementing liquid system and preparation and application methods thereof |
| CN112456955B (en) * | 2020-12-01 | 2022-06-03 | 西南科技大学 | Basic magnesium sulfate cement-based lightweight porous material and preparation method thereof |
| CN113772978B (en) * | 2021-10-20 | 2022-11-01 | 辽宁科技大学 | Method for preparing composite magnesium oxysulfate cement capable of being constructed in winter by using desulfurization solution |
| CN114634348B (en) * | 2022-04-25 | 2022-08-30 | 江苏正方园建设集团有限公司 | Environment-friendly magnesium oxysulfate material production process and magnesium oxysulfate plate |
| CN114890769A (en) * | 2022-05-27 | 2022-08-12 | 韩涛 | Self-leveling heat-conducting cementing material and preparation method and application thereof |
| CN115636655B (en) * | 2022-07-26 | 2024-03-26 | 国网山东省电力公司电力科学研究院 | High-fluidity self-compaction light high-strength concrete and preparation method thereof |
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| CN103130436A (en) * | 2013-03-25 | 2013-06-05 | 中国科学院上海硅酸盐研究所 | Oxidized graphene and graphene reinforced cement based composite material and preparation method thereof |
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