CN112919484A - Magnesium silicate prepared by taking quartz sand as siliceous raw material and method thereof - Google Patents
Magnesium silicate prepared by taking quartz sand as siliceous raw material and method thereof Download PDFInfo
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Abstract
The invention discloses a magnesium silicate prepared by taking quartz sand as a siliceous raw material and a method thereof, wherein the magnesium silicate is prepared from the following raw materials: 60-69 parts of quartz sand, 40-55 parts of magnesium oxide and water; the water-solid ratio is 0.20-0.50. In the method, quartz is used as a siliceous raw material to replace silica fume, and the hydrated magnesium silicate gel can be prepared under the conditions of high temperature and high pressure. The quartz comprises SiO as main component2Compared with silica fume, the silica fume has high crystallinity and stable chemical property. In the experiment, the high-temperature and high-pressure conditions of 160-200 ℃ and 0.62-1.55 MPa pressure are adopted, and the reaction is promoted by improving the activation energy of the reaction, so that the hydrated magnesium silicate gel is prepared.
Description
Technical Field
The invention belongs to the technical field of magnesium silicate, and particularly relates to magnesium silicate prepared by taking quartz as a siliceous raw material and active magnesium oxide under a steam-curing condition and a method thereof.
Background
The cement is the most used inorganic cementing material in the world, and the cement product is applied to every corner of economic construction, thereby becoming the basis of the development of human society. However, the production of conventional portland cement on a large scale creates an incompatibility between the development of the conventional cement industry and the resources and environments. According to statistics, CO of cement production2The emission of CO accounts for the whole world27% of the discharge, in addition, the requirement of a large amount of aggregates in the concrete preparation process causes a large amount of exploitation of resources, and according to statistics of relevant departments, the concrete is currently consuming natural aggregates at a rate of about 70 hundred million tons per year as the largest consumer of natural resources such as water, sand, pebbles, broken stones and the like. This forces intensive research and comprehensive optimization of the production and use of conventional cements, and also requires the development and exploitation of new cement materials.
The magnesium mineral resources in China are rich, but in the traditional calcium cement, the quality of the cement can be influenced by the existence of MgO, and if people can utilize idle magnesium mineral resources and magnesium-containing wastes in China to prepare a novel magnesium cementing material capable of replacing the calcium cement, great contribution can be made to the goals of protecting the environment, utilizing the resources and realizing sustainable development. Over 100 years ago, the concept of hydrated magnesium silicate cements became apparent. In the 90 s of the 19 th century, the product of magnesite after calcination and silica fume are mixed and reacted to prepare the hydrated magnesium silicate with gelling capacity. At the end of the 19 th century, Steiger prepared this new cement by mixing magnesium chloride, magnesium oxide, sodium silicate and water. Subsequently, in several monographs, cements of the magnesium oxychloride type and granulated asbestos as well as readily soluble silicic acids were used to prepare the cement, as well as talc/asbestos and modified-nature activated SiO2The prepared refractory mass, but more systematic studies on the hydrated magnesium silicate gelling system have not been performed.
MgO-SiO prepared in the last two decades2-H2The O (M-S-H) gel system is prepared by reacting active magnesium oxide or magnesium hydroxide with high-activity siliceous raw materials (silica fume, slag, fly ash and the like) to obtain MgO-SiO2-H2And (3) an O gelling system. Preparation of MgO-SiO by using magnesium oxide and silica fume for Wenjiang et al2-H2O-gel system, and MgO-SiO prepared at different Mg/Si ratios and different temperatures2-H2The O-gelling system was studied initially. The results show that: the specific surface area of the silica fume of the gel system is largeThe water demand is large, so that the water demand of the system is reduced by modifying the system by adding a dispersing agent, a surfactant and the like. Wenjiang et al tried various dispersants and found that sodium hexametaphosphate (Na-HMP) was on MgO-SiO2-H2The modification effect of the O system is the best. In addition, Cheeseman and baiting et al made systematic studies on the changes in the shrinkage of M-S-H gels and the change in pH of M-S-H gel systems.
Zhang Ting et al according to MgO-SiO2-H2The O-gel system has low pH value and good wrapping capacity, and the MgO-SiO with lower alkalinity (9.5-10.5) is prepared by utilizing active magnesium oxide and high-activity silica fume2-H2The O-cement is used to cure nuclear waste and the system is applied to a low pH sprayed cement mortar for curing and a matrix containing metallic aluminum nuclear waste. MgO-SiO in comparison with conventional portland cement2-H2The low basicity of the O-cement makes it non-halogenous, but not suitable for reinforced concrete.
Although active MgO, silica fume (SiO) is used at present2) And a proper amount of water to prepare MgO-SiO2-H2The O-gelling system is a common method, however, the pure siliceous raw materials such as silica fume and the like have limited sources and are relatively high in price, so that the cost for preparing the hydrated magnesium silicate material is correspondingly high. Therefore, in order to reduce the preparation cost and have excellent mechanical properties, the fly ash is used by Doctorian and the like to replace part of silica fume to prepare the hydrated magnesium silicate cement, and the compression strength, the setting time, the dry shrinkage and the microstructure of the hydrated magnesium silicate cement are tested and researched. The mixing amount of the magnesium oxide, the fly ash and the silica fume, the using amount of the sodium hexametaphosphate and the reasonable water-cement ratio are determined through a series of experiments, and the maximum compression strength of the prepared hydrated magnesium silicate cement can reach 47MPa after the hydrated magnesium silicate cement is maintained for a period of time, so that the basic requirement on the compression strength in engineering can be met.
Disclosure of Invention
In view of the problems in the prior art, the invention provides magnesium silicate prepared by taking quartz sand as a siliceous raw material and a method thereof.
The invention provides a method for preparing magnesium silicate by taking quartz sand as a siliceous raw material, which comprises the following specific steps:
the method comprises the following steps: and (3) grinding, namely grinding the quartz sand to a middle position with the diameter of 7.937-27.477 mu m (the equipment in the prior art such as a ball mill, a vibration mill, an air flow mill and the like can be adopted).
Step two: weighing a certain mass of active magnesium oxide and quartz powder according to a specific experimental proportion, and putting the active magnesium oxide and the quartz powder into a clean slurry stirrer for dry stirring for 2-3 min to uniformly mix the raw materials; and pouring weighed water while stirring after dry stirring, and quickly stirring in a neat paste stirrer for 2-4 min.
Step three: and pouring the slurry which is uniformly stirred into a mold with a certain size quickly, and vibrating on a vibrating table for 60-120 seconds to obtain a sample.
Step four: and (4) putting the sample belt mold prepared in the third step into a steam curing box, and pre-curing for 4-8 hours at the temperature of 50-70 ℃.
Step five: and when the precuring time is finished and the temperature is reduced to the room temperature, taking out the die, removing the die, then discharging the die into the autoclave, carrying out steam curing for 6-10 h at the temperature of 160-200 ℃, and taking out the die after the temperature is reduced to the room temperature.
The preparation method comprises the following raw materials in parts by weight: 45-69 parts of quartz sand and 31-55 parts of magnesium oxide. The weight of water can be increased or decreased according to the mixing amount of the water reducing agent, and the water is moderate (the water-solid ratio ranges from 0.30 to 0.50).
The preparation method is used for preparing SiO in quartz sand2Content (wt.)>92％。
In the preparation method, the granularity of the quartz sand needs to be ground to a median diameter of 7.937-27.477 mu m.
The magnesium oxide prepared by the preparation method is active magnesium oxide with MgO content of more than 90%.
The preparation method of the magnesium silicate cementing material comprises MgO/SiO2The molar ratio is between 0.67 and 1.83 (the mass ratio is between 0.45 and 0.89).
In the method, quartz is used as a siliceous raw material to replace silica fume, and the hydrated magnesium silicate gel can be prepared under the conditions of high temperature and high pressure. The quartz comprises SiO as main component2Compared with the silicon ash, the silicon ash has the advantages that,it has high crystallinity and stable chemical property. In the experiment, the high-temperature and high-pressure conditions of 160-200 ℃ and 0.62-1.55 MPa pressure are adopted, and the reaction is promoted by improving the activation energy of the reaction, so that the hydrated magnesium silicate gel is prepared.
Drawings
FIG. 1 shows MgO-SiO-prepared in examples 3 and 4 with Mg/Si molar ratios of 1.33 and 1.502-H2X-ray diffraction pattern of the O-gel system at 3d age.
FIG. 2 shows MgO-SiO prepared in examples 3 and 4 when the molar ratio of Mg/Si is 1.33 and 1.502-H2And (3) a micro-topography of the O-gel system at the age of 3 d.
Detailed Description
The present invention will be described in detail with reference to specific examples.
The preparation process of the invention comprises the following steps (the preparation process of each example is based on the following steps):
the method comprises the following steps: and (3) grinding, namely grinding the quartz sand to a middle position with the diameter of 7.937-27.477 mu m (the equipment in the prior art such as a ball mill, a vibration mill, an air flow mill and the like can be adopted).
Step two: weighing a certain mass of active magnesium oxide and ground quartz powder according to an experimental ratio, and putting the active magnesium oxide and the ground quartz powder into a clean slurry stirrer for dry stirring for 2-3 min to uniformly mix the raw materials; and pouring weighed water while stirring after dry stirring, and quickly stirring in a neat paste stirrer for 2-4 min.
Step three: and quickly pouring the uniformly stirred slurry into a mold with a certain size, and vibrating on a vibrating table for 60-120 seconds to obtain a sample.
Step four: and (5) putting the sample belt mold obtained in the step two into a steam curing box, and pre-curing for 4-8 hours at the temperature of 50-70 ℃.
Step five: and after the precuring time is finished and the temperature is reduced to the room temperature, taking out the mold, removing the mold, then discharging the mold into the autoclave, performing steam curing for 6-10 hours at the temperature of 160-200 ℃, and taking out the mold after cooling.
Example 1
The magnesium silicate system gelled material prepared based on quartz sand and active magnesium oxide in the embodiment comprises the following raw materials: 40 parts of quartz sand, 60 parts of active magnesium oxide and 0.5 of water-solid ratio.
The preparation method of the magnesium silicate system gel material based on quartz powder and active magnesium oxide includes the following steps:
the method comprises the following steps: and (3) grinding, namely grinding the quartz sand to the median diameter of 7.937 mu m.
Step two: weighing a certain mass of active magnesium oxide and ground quartz powder according to an experimental ratio, and putting the active magnesium oxide and the ground quartz powder into a clean slurry stirrer for dry stirring for 2min to uniformly mix the raw materials; after dry stirring, pouring weighed water while stirring, and quickly stirring in a pure slurry stirrer for 3 min.
Step three: quickly pouring the uniformly stirred slurry into a 30 x 30mm container2And vibrated on a vibrating table for 60 seconds to produce a sample.
Step four: and (4) putting the sample block with the mold obtained in the step three into a steam curing box, and pre-curing for 6 hours at the temperature of 60 ℃.
Step five: and after the pre-curing time is finished and the temperature is reduced to the room temperature, taking out the mold, removing the mold, putting the test block into a high-temperature reaction kettle, sealing the autoclave kettle, turning on a power supply, raising the temperature of the autoclave kettle from the room temperature to 200 ℃, and autoclaving the test block in the autoclave kettle at the autoclaving temperature of 200 ℃ and the pressure of 1.55MPa for 10 hours. After the autoclave is cooled, the test block is taken out, and then the test block is continuously maintained in a constant temperature and humidity box with the temperature of 20 ℃ and the temperature of 2 ℃ and the humidity of more than 95 percent until the test block reaches the specified age.
Example 2
The magnesium silicate system gelled material prepared based on quartz sand and active magnesium oxide in the embodiment comprises the following raw materials: 56.2 parts of quartz sand, 43.8 parts of active magnesium oxide and 0.5 of water-solid ratio.
The preparation method of the magnesium silicate system gel material based on quartz powder and active magnesium oxide includes the following steps:
the method comprises the following steps: and (3) grinding, namely grinding the quartz sand to the median diameter of 7.937 mu m.
Step two: weighing a certain mass of active magnesium oxide and ground quartz powder according to an experimental ratio, and putting the active magnesium oxide and the ground quartz powder into a clean slurry stirrer for dry stirring for 2min to uniformly mix the raw materials; after dry stirring, pouring weighed water while stirring, and quickly stirring in a pure slurry stirrer for 3 min.
Step three: quickly pouring the uniformly stirred slurry into a 30 x 30mm container2And vibrated on a vibrating table for 60 seconds to produce a sample.
Step four: and (4) putting the sample block with the mold obtained in the step three into a steam curing box, and pre-curing for 6 hours at the temperature of 60 ℃.
Step five: and after the pre-curing time is finished and the temperature is reduced to the room temperature, taking out the mold, removing the mold, putting the test block into a high-temperature reaction kettle, sealing the autoclave kettle, turning on a power supply, raising the temperature of the autoclave kettle from the room temperature to 200 ℃, and autoclaving the test block in the autoclave kettle at the autoclaving temperature of 200 ℃ and the pressure of 1.55MPa for 10 hours. After the autoclave is cooled, the test block is taken out, and then the test block is continuously maintained in a constant temperature and humidity box with the temperature of 20 ℃ and the temperature of 2 ℃ and the humidity of more than 95 percent until the test block reaches the specified age.
Example 3
The magnesium silicate system gelled material prepared based on quartz sand and active magnesium oxide in the embodiment comprises the following raw materials: 53 parts of quartz sand, 47 parts of active magnesium oxide and 0.5 of water-solid ratio.
The preparation method of the magnesium silicate system gel material based on quartz powder and active magnesium oxide includes the following steps:
the method comprises the following steps: and (3) grinding, namely grinding the quartz sand to the median diameter of 7.937 mu m.
Step two: weighing a certain mass of active magnesium oxide and ground quartz powder according to an experimental ratio, and putting the active magnesium oxide and the ground quartz powder into a clean slurry stirrer for dry stirring for 2min to uniformly mix the raw materials; after dry stirring, pouring weighed water while stirring, and quickly stirring in a pure slurry stirrer for 3 min.
Step three: quickly pouring the uniformly stirred slurry into a 30 x 30mm container2And vibrated on a vibrating table for 60 seconds to produce a sample.
Step four: and (4) putting the sample block with the mold obtained in the step three into a steam curing box, and pre-curing for 6 hours at the temperature of 60 ℃.
Step five: and after the pre-curing time is finished and the temperature is reduced to the room temperature, taking out the mold, removing the mold, putting the test block into a high-temperature reaction kettle, sealing the autoclave kettle, turning on a power supply, raising the temperature of the autoclave kettle from the room temperature to 200 ℃, and autoclaving the test block in the autoclave kettle at the autoclaving temperature of 200 ℃ and the pressure of 1.55MPa for 10 hours. After the autoclave is cooled, the test block is taken out, and then the test block is continuously maintained in a constant temperature and humidity box with the temperature of 20 ℃ and the temperature of 2 ℃ and the humidity of more than 95 percent until the test block reaches the specified age.
Example 4
The magnesium silicate system gelled material prepared based on quartz sand and active magnesium oxide in the embodiment comprises the following raw materials: 50 parts of quartz sand, 50 parts of active magnesium oxide and 0.5 of water-solid ratio.
The preparation method of the magnesium silicate system gel material based on quartz powder and active magnesium oxide includes the following steps:
the method comprises the following steps: and (3) grinding, namely grinding the quartz sand to the median diameter of 7.937 mu m.
Step two: weighing a certain mass of active magnesium oxide and ground quartz powder according to an experimental ratio, and putting the active magnesium oxide and the ground quartz powder into a clean slurry stirrer for dry stirring for 2min to uniformly mix the raw materials; after dry stirring, pouring weighed water while stirring, and quickly stirring in a pure slurry stirrer for 3 min.
Step three: quickly pouring the uniformly stirred slurry into a 30 x 30mm container2And vibrated on a vibrating table for 60 seconds to produce a sample.
Step four: and (4) putting the sample block with the mold obtained in the step three into a steam curing box, and pre-curing for 6 hours at the temperature of 60 ℃.
Step five: and after the pre-curing time is finished and the temperature is reduced to the room temperature, taking out the mold, removing the mold, putting the test block into a high-temperature reaction kettle, sealing the autoclave kettle, turning on a power supply, raising the temperature of the autoclave kettle from the room temperature to 200 ℃, and autoclaving the test block in the autoclave kettle at the autoclaving temperature of 200 ℃ and the pressure of 1.55MPa for 10 hours. After the autoclave is cooled, the test block is taken out, and then the test block is continuously maintained in a constant temperature and humidity box with the temperature of 20 ℃ and the temperature of 2 ℃ and the humidity of more than 95 percent until the test block reaches the specified age.
Example 5
The magnesium silicate system gelled material prepared based on quartz sand and active magnesium oxide in the embodiment comprises the following raw materials: 60 parts of quartz sand, 40 parts of active magnesium oxide and 0.5 of water-solid ratio.
The preparation method of the magnesium silicate system gel material based on quartz powder and active magnesium oxide includes the following steps:
the method comprises the following steps: and (3) grinding, namely grinding the quartz sand to the median diameter of 27.477 mu m.
Step two: weighing a certain mass of active magnesium oxide and ground quartz powder according to an experimental ratio, and putting the active magnesium oxide and the ground quartz powder into a clean slurry stirrer for dry stirring for 2min to uniformly mix the raw materials; after dry stirring, pouring weighed water while stirring, and quickly stirring in a pure slurry stirrer for 3 min.
Step three: quickly pouring the uniformly stirred slurry into a 30 x 30mm container2And vibrated on a vibrating table for 60 seconds to produce a sample.
Step four: and (4) putting the sample block with the mold obtained in the step three into a steam curing box, and pre-curing for 6 hours at the temperature of 60 ℃.
Step five: and after the pre-curing time is finished and the temperature is reduced to the room temperature, taking out the mold, removing the mold, putting the test block into a high-temperature reaction kettle, sealing the autoclave kettle, turning on a power supply, raising the temperature of the autoclave kettle from the room temperature to 200 ℃, and autoclaving the test block in the autoclave kettle at the autoclaving temperature of 200 ℃ and the pressure of 1.55MPa for 10 hours. After the autoclave is cooled, the test block is taken out, and then the test block is continuously maintained in a constant temperature and humidity box with the temperature of 20 ℃ and the temperature of 2 ℃ and the humidity of more than 95 percent until the test block reaches the specified age.
Example 6
The magnesium silicate system gelled material prepared based on quartz sand and active magnesium oxide in the embodiment comprises the following raw materials: 50 parts of quartz sand, 50 parts of active magnesium oxide and 0.3 of water-solid ratio.
The preparation method of the magnesium silicate system gel material based on quartz powder and active magnesium oxide includes the following steps:
the method comprises the following steps: and (3) grinding, namely grinding the quartz sand to the median diameter of 7.937 mu m.
Step two: weighing a certain mass of active magnesium oxide and ground quartz powder according to an experimental ratio, and putting the active magnesium oxide and the ground quartz powder into a clean slurry stirrer for dry stirring for 2min to uniformly mix the raw materials; after dry mixing, the water reducing agent and the water which are weighed in advance are poured in turn while stirring, and the mixture is quickly stirred for 4min in a paste cleaning stirrer.
Step three: quickly pouring the uniformly stirred slurry into a 30 x 30mm container2And vibrated on a vibrating table for 60 seconds to produce a sample.
Step four: and (4) putting the sample block with the mold obtained in the step three into a steam curing box, and pre-curing for 6 hours at the temperature of 60 ℃.
Step five: and after the pre-curing time is finished and the temperature is reduced to the room temperature, taking out the mold, removing the mold, putting the test block into a high-temperature reaction kettle, sealing the autoclave kettle, turning on a power supply, raising the temperature of the autoclave kettle from the room temperature to 200 ℃, and autoclaving the test block in the autoclave kettle at the autoclaving temperature of 200 ℃ and the pressure of 1.55MPa for 8 hours. After the autoclave is cooled, the test block is taken out, and then the test block is continuously maintained in a constant temperature and humidity box with the temperature of 20 ℃ and the temperature of 2 ℃ and the humidity of more than 95 percent until the test block reaches the specified age.
FIG. 1 is an X-ray diffraction pattern of the M-S-H gel system prepared at 3d age for Mg/Si molar ratios of 1.33 and 1.50 in examples 3 and 4. As can be seen from the figure, when the Mg/Si molar ratio is 1.33 and 1.50, the steamed bun peaks of M-S-H were observed at 2 theta angles of 10-14 °, 22-26 °, 34-38 ° and 58-62 °, and no Mg (OH)2The presence of a peak indicating Mg (OH) formed by hydration of active magnesium oxide2With SiO2Fully reacting to generate hydrated magnesium silicate gel. In addition, SiO with a weaker strength was found in the graph at a Mg/Si molar ratio of 1.33 as compared with a molar ratio of 1.502Crystallization peak.
FIG. 2 shows MgO-SiO-prepared in examples 3 and 4 with Mg/Si molar ratios of 1.33 (FIG. a) and 1.50 (FIG. b)2-H2And (3) a micro-topography of the O-gel system at the age of 3 d. As can be seen, the active magnesium oxide and the ground quartz sand form a compact structure of hydrated magnesium silicate gel under autoclaving conditions.
The above examples tested the compressive strength of test blocks with different Mg/Si molar ratios (1.0, 1.18, 1.33, 1.5) after curing for 4 ages of 3d, 28d, 90d and 180d, 6 test blocks were proportioned to each test block, and the average of the 6 test blocks was used as the experimental result, and the standard deviation was calculated.
TABLE 1
As can be seen from the table, the compressive strength of the test block is increased along with the increase of the Mg/Si molar ratio, and the maximum compressive strength value can reach about 23 MPa. This shows that as the molar ratio of Mg/Si increases, the amounts of MgO and SiO2 obtained in the system are sufficient, and the MgO and the SiO2 can completely react to form hydrated magnesium silicate gel with a denser structure, so that the compressive strength of the test block is improved. The data in Table 1 show that the change of Mg/Si molar ratio has a larger influence on the strength, and from the law of development and change of strength at 4 ages, the strength of the generated hydrated magnesium silicate is better when the Mg/Si molar ratio is 1.33 and 1.5, and can reach 22.2MPa and 23.5 MPa.
In the above examples and in the present specification, the percentages which are not specified are by weight, and the steps and processes which are not specifically recited are equivalent to the prior art.
The present invention is not limited to the above-described embodiments, and the present invention can be implemented with the above-described advantageous effects.
It will be understood that modifications and variations can be made by persons skilled in the art in light of the above teachings and all such modifications and variations are intended to be included within the scope of the invention as defined in the appended claims.
Claims (7)
1. A method for preparing magnesium silicate by taking quartz sand as a siliceous raw material is characterized in that the raw material for preparing the magnesium silicate comprises the following components: 60-69 parts of quartz sand, 40-55 parts of magnesium oxide and water; the water-solid ratio is 0.20-0.50.
2. The magnesium silicate material of claim 1, wherein said silica sand is a normal silica sand, and SiO is contained in said silica sand2Content (wt.)>92％。
3. The method as claimed in claim 1, wherein the median diameter of the silica sand is 7.937-27.477 μm.
4. The method according to claim 1, characterized in that the magnesium oxide is activated magnesium oxide with a MgO content > 90%.
5. The method of claim 1, wherein the magnesium silicate cement is MgO/SiO thereof2The molar ratio is between 0.67 and 1.83.
6. The method according to claim 1, characterized in that it comprises in particular the steps of:
the method comprises the following steps: grinding, namely grinding the quartz sand to a median diameter of 7.937-27.477 mu m;
step two: weighing a certain mass of active magnesium oxide and ground quartz powder according to an experimental ratio, and putting the active magnesium oxide and the ground quartz powder into a clean slurry stirrer for dry stirring for 2-3 min to uniformly mix the raw materials; pouring weighed water while stirring after dry stirring, and quickly stirring in a neat paste stirrer for 2-4 min;
step three: quickly pouring the uniformly stirred slurry into a mold with a certain size, and vibrating on a vibrating table for 60-120 seconds to obtain a sample;
step four: putting the sample belt mold obtained in the step three into a steam curing box, and pre-curing for 4-8 hours at the temperature of 50-70 ℃;
step five: and (3) taking out the mold for mold stripping when the pre-curing time is finished and the temperature is reduced to the room temperature, then putting the test block subjected to mold stripping into an autoclave, performing steam curing for 6-10 h under the conditions of 160-200 ℃ and 0.62-1.55 MPa, and taking out after cooling.
7. Magnesium silicate produced by the process of any one of claims 1 to 6.
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