CN111646723A - High-content concrete activator and preparation method thereof - Google Patents
High-content concrete activator and preparation method thereof Download PDFInfo
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- CN111646723A CN111646723A CN202010380903.2A CN202010380903A CN111646723A CN 111646723 A CN111646723 A CN 111646723A CN 202010380903 A CN202010380903 A CN 202010380903A CN 111646723 A CN111646723 A CN 111646723A
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- 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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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Abstract
The invention discloses a high-content concrete activator and a preparation method thereof, belonging to the technical field of building materials. A high-content concrete activator is prepared from the following raw materials in percentage by weight: 30-40% of alkaline residue, 15-25% of ammonium nitrate solution, 10-20% of quartz sand tailings, 10-20% of gypsum and 15-25% of reinforcing agent. The invention has the beneficial effects that: the coagulation and hardening of the slag concrete with large mixing amount are accelerated, so that the coagulation time and the early strength of the slag concrete are almost the same as those of common concrete, and the construction is convenient. Compared with the prior methods of mechanical activation, chemical excitation and the like, the method avoids redundant energy consumption and avoids side effects on later-period performance. The raw materials mostly adopt solid waste materials, and a new channel is provided for the development and utilization of the solid waste.
Description
Technical Field
The invention relates to a high-content concrete activator and a preparation method thereof, belonging to the technical field of building materials.
Background
With the development of industrial production, the amount of industrial waste is increasing. Especially the largest industrial discharge amount of metallurgy, thermal power generation and the like. The industrial waste is large in quantity, various in types, complex in components and quite difficult to treat. Today, only a limited number of industrial wastes are utilized, such as steel slag in the united states, sweden, etc., and fly ash and coal slag in japan, denmark, etc. Other industrial wastes are mainly stored in a passive manner, and part of harmful industrial solid wastes are treated by methods such as landfill, incineration, chemical conversion, microbial treatment and the like; some are thrown into the ocean. The passive stockpiling of industrial wastes not only occupies a large amount of land and causes the waste of manpower and material resources, but also a lot of industrial waste residues contain substances which are easy to dissolve in water and pollute soil and water bodies through leaching. Powdery industrial wastes fly with wind, pollute the atmosphere, and emit odor and toxic gases. Some wastes even foul the river channel, pollute the water system, influence the growth of organisms and harm the health of human bodies. Therefore, secondary development, utilization and research on industrial solid wastes are in great tendency and urgent need.
At present, the treatment mode of industrial solid waste in China mainly comprises the following aspects of (1) extracting and recovering valuable (rare) metals in metallurgical waste residues, and changing waste into valuables. Because of the extensive economy in China for a long time, only much attention is paid to the recovery of main metals in the resource exploitation process, so that a large amount of valuable metals and associated metals still remain in metallurgical wastes, and a large amount of potential resource loss and ecological environment damage are caused. Therefore, the extraction of the valuable (rare) metals is an important way for realizing the utilization of solid wastes as resources. However, the disposal mode causes secondary pollution to the environment, and the comprehensive utilization rate of solid wastes cannot be obviously improved, (2) mine goaf filling is carried out. At present, in order to realize resource utilization of industrial solid wastes, industrial solid wastes are used for landfill in mining dead areas in many medium and small cities, so that the land surface collapse of the mining dead areas can be prevented, and the ecological environment of China can be improved. But the mining area of China is limited, the landfill cost is higher, and the development of circular economy is not facilitated, (3) chemical conversion and microbial treatment methods. The method has quite limited application range before the industrial solid waste containing toxic substances such as sulfur, mercury, cadmium and the like is not treated, and can firstly carry out chemical conversion and microbial treatment to enlarge the application range, even if the method can solve the environmental problem caused by the industrial solid waste to a certain extent, the method cannot radically reduce the stockpiling amount of waste residues, and (4) produce novel building materials. After being cooled, a plurality of metallurgical slags have higher activity and strength, and can be directly used as cementing materials, cementing material components, wall aggregates, mineral admixtures, high-quality aggregates of high-performance concrete and the like after being crushed or water quenched. With the development of the building industry and the emerging industry in China, the application approach with high added value is undoubtedly the best choice for best consuming industrial solid waste, and the development of building materials not only greatly improves the utilization space of industrial solid waste, but also fundamentally solves the problem of the coordinated development of energy and environment in China.
Slag has been widely used in the production of modern concrete. With the increasingly prominent requirements on effective energy conservation, reasonable resource utilization and ecological environment protection, research and application of using high-doped slag (more than 50%) in a portland cement concrete system are increasing. However, the high-content slag concrete has a relatively limited cement content, so that the early mechanical properties of the concrete are slowly developed and are often limited in engineering application.
In the process of research, some scholars find that the early reaction activity of the slag can be improved by mechanical activation, chemical excitation and the like. However, the mechanical activation method is to refine slag particles, increase a hydration reaction interface and promote slag reaction on the premise of sacrificing energy consumption. The chemical excitation method is mainly characterized in that alkaline substances or sulfate and other components are added into the slag to rapidly excite the potential activity of the slag, and the alkaline substances or sulfate mainly aim at an alkaline slag gelling system; the latter must be in alkaline environment to fully play the role of sulfate activity excitation, and the hydration activity of the gelling system is excited by only sulfate, which may cause the phenomena of abnormal setting time, late strength shrinkage and the like of concrete. Therefore, it is still a topic worth systematic study to adopt appropriate methods to promote the development of early strength of cement-highly doped slag systems without affecting later performance.
The alkaline residue is the waste residue discharged in the process of preparing alkali by an ammonia-soda process. The ammonia-soda process for preparing alkali in China can reach 421 ten thousand t/year. Due to the characteristics of the ammonia-soda process soda ash production process, 0.3 t of caustic sludge needs to be discharged outwards when 1 t of soda ash is produced, and the cost for waste residue discharge is about 1000 ten thousand yuan every year in a factory producing 80 ten thousand of soda ash every year. In general, the caustic sludge is processed by surface accumulation, and a large amount of caustic sludge is deposited to form a piece of 'white sea', which causes pollution to surrounding sea areas. Therefore, the alkaline residue is effectively utilized, waste is changed into valuable, and the method has obvious social benefit and economic benefit and broad prospect.
The quartz sand tailings are waste which is inevitably generated in the process of sand ore dressing purification and fine and further processing. According to statistics, nearly 4000 million tons of quartz sand tailings are produced every year in China, a large amount of quartz sand tailings occupy land, pollute the environment, and a lot of enterprises are penalized or shut down due to the fine. Along with the coming and implementing of the environmental protection tax law and the gradual and severe situation of policies such as environmental protection, safety and the like, the problem of comprehensive utilization of the quartz sand tailings is increasingly prominent. The quartz tailings comprise waste residues in ore mining, tailings and tailings in the processing process, wherein the tailings account for the vast majority. The chemical components of the quartz tailings are mainly SiO2, the impurities are mainly feldspar, clay, mica, iron minerals and the like, and the quartz tailings can eliminate pollution, change waste into valuable, widen the application range of mineral products, improve the additional value of the mineral products and have wide development prospect as long as reasonable development and scientific utilization are realized.
Disclosure of Invention
In order to solve the technical problems, the invention provides a high-content concrete activator and a preparation method thereof, which can effectively solve the problems of setting time, early strength and the like.
The technical scheme adopted by the invention is as follows:
a high-content concrete activator is prepared from the following raw materials in percentage by weight: 30-40% of alkaline residue, 15-25% of ammonium nitrate solution, 10-20% of quartz sand tailings, 10-20% of gypsum and 15-25% of reinforcing agent.
Further, the material is prepared from the following raw materials in percentage by weight: 35% of alkaline residue, 25% of ammonium nitrate solution, 15% of quartz sand tailings, 10% of gypsum and 15% of reinforcing agent.
Further, the caustic sludge comprises the following main components in percentage by weight: 60-65% of calcium carbonate, 10-15% of calcium chloride and 15-28% of calcium hydroxide, wherein the particle size of the alkaline residue is not more than 75 μm, and the used alkaline residue is dechlorinated alkaline residue with the chlorine content of less than 0.3%.
Further, the quartz sand tailings comprise the following main components in percentage by weight: 90-99% of silicon dioxide, and the particle size is not more than 75 μm.
Further, the concentration of the sodium nitrate solution is 35%.
Further, the reinforcing agent is triethanolamine.
A method for preparing the high loading concrete activator of claim 1, comprising the steps of:
grinding the dechlorinated alkaline residues, and controlling the particle size to be 40-80 mm;
placing the ground caustic sludge in a calcining kiln, calcining at 900-1200 ℃ for 40-60 minutes, cooling to obtain calcium oxide, selecting the calcium oxide, adding water for digestion, purifying, drying and sieving to obtain calcium hydroxide powder;
adding calcium hydroxide powder into 35% ammonium nitrate solution, mixing, heating in water bath, stirring, continuously supplementing evaporated water until ammonia smell is small, stopping heating, filtering, washing with water, and precipitating to obtain calcium nitrate tetrahydrate;
step four, further selecting the quartz sand tailings to enable the content of silicon dioxide to reach more than 99%;
and step five, mixing and stirring the calcium nitrate tetrahydrate, the carefully selected quartz sand tailings, the gypsum and the reinforcing agent to obtain the activating agent.
The invention has the beneficial effects that:
the coagulation and hardening of the slag concrete with large mixing amount are accelerated, so that the coagulation time and the early strength of the slag concrete are almost the same as those of common concrete, and the construction is convenient. Compared with the prior methods of mechanical activation, chemical excitation and the like, the method avoids redundant energy consumption and avoids side effects on later-period performance. The raw materials mostly adopt solid waste materials, and a new channel is provided for the development and utilization of the solid waste.
Detailed Description
The materials, methods and apparatus used in the following examples, which are not specifically illustrated, are conventional in the art and are commercially available to those of ordinary skill in the art.
In addition, in the following description of the present invention, the meaning of "plurality", and "plural" is two or more unless otherwise specified.
The present invention is described in further detail below, but the following detailed description is not to be construed as limiting the invention.
Example 1
A high-content concrete activator is prepared from the following raw materials in percentage by weight: 35% of alkaline residue, 25% of ammonium nitrate solution, 15% of quartz sand tailings, 10% of gypsum and 15% of reinforcing agent. The caustic sludge comprises the following main components in percentage by weight: 60-65% of calcium carbonate, 10-15% of calcium chloride and 15-28% of calcium hydroxide, wherein the particle size of the alkaline residue is not more than 75 μm, and the used alkaline residue is dechlorinated alkaline residue with the chlorine content of less than 0.3%. The quartz sand tailings comprise the following main components in percentage by weight: 90-99% of silicon dioxide, and the particle size is not more than 75 μm. The concentration of the sodium nitrate solution is 35%. The reinforcing agent is triethanolamine.
A method for preparing the high loading concrete activator of claim 1, comprising the steps of:
grinding the dechlorinated alkaline residues, and controlling the particle size to be 40-80 mm;
placing the ground caustic sludge in a calcining kiln, calcining at 900-1200 ℃ for 40-60 minutes, cooling to obtain calcium oxide, selecting the calcium oxide, adding water for digestion, purifying, drying and sieving to obtain calcium hydroxide powder;
adding calcium hydroxide powder into 35% ammonium nitrate solution, mixing, heating in water bath, stirring, continuously supplementing evaporated water until ammonia smell is small, stopping heating, filtering, washing with water, and precipitating to obtain calcium nitrate tetrahydrate;
step four, further selecting the quartz sand tailings to enable the content of silicon dioxide to reach more than 99%;
and step five, mixing and stirring the calcium nitrate tetrahydrate, the carefully selected quartz sand tailings, the gypsum and the reinforcing agent to obtain the activating agent.
Example 2
A high-content concrete activator is prepared from the following raw materials in percentage by weight: 40% of alkaline residue, 10% of ammonium nitrate solution, 10% of quartz sand tailings, 15% of gypsum and 25% of reinforcing agent. The caustic sludge comprises the following main components in percentage by weight: 60-65% of calcium carbonate, 10-15% of calcium chloride and 15-28% of calcium hydroxide, wherein the particle size of the alkaline residue is not more than 75 μm, and the used alkaline residue is dechlorinated alkaline residue with the chlorine content of less than 0.3%. The quartz sand tailings comprise the following main components in percentage by weight: 90-99% of silicon dioxide, and the particle size is not more than 75 μm. The concentration of the sodium nitrate solution is 35%. The reinforcing agent is triethanolamine.
A method for preparing the high loading concrete activator of claim 1, comprising the steps of:
grinding the dechlorinated alkaline residues, and controlling the particle size to be 40-80 mm;
placing the ground caustic sludge in a calcining kiln, calcining at 900-1200 ℃ for 40-60 minutes, cooling to obtain calcium oxide, selecting the calcium oxide, adding water for digestion, purifying, drying and sieving to obtain calcium hydroxide powder;
adding calcium hydroxide powder into 35% ammonium nitrate solution, mixing, heating in water bath, stirring, continuously supplementing evaporated water until ammonia smell is small, stopping heating, filtering, washing with water, and precipitating to obtain calcium nitrate tetrahydrate;
step three, further selecting the quartz sand tailings to enable the content of silicon dioxide to reach more than 99%;
and step four, mixing and stirring the calcium nitrate tetrahydrate, the carefully selected quartz sand tailings, the gypsum and the reinforcing agent to obtain the activating agent.
Example 3
A high-content concrete activator is prepared from the following raw materials in percentage by weight: 30% of alkaline residue, 20% of ammonium nitrate solution, 10% of quartz sand tailings, 20% of gypsum and 20% of reinforcing agent. The caustic sludge comprises the following main components in percentage by weight: 60-65% of calcium carbonate, 10-15% of calcium chloride and 15-28% of calcium hydroxide, wherein the particle size of the alkaline residue is not more than 75 μm, and the used alkaline residue is dechlorinated alkaline residue with the chlorine content of less than 0.3%. The quartz sand tailings comprise the following main components in percentage by weight: 90-99% of silicon dioxide, and the particle size is not more than 75 μm. The concentration of the sodium nitrate solution is 35%. The reinforcing agent is triethanolamine.
A method for preparing the high loading concrete activator of claim 1, comprising the steps of:
grinding the dechlorinated alkaline residues, and controlling the particle size to be 40-80 mm;
placing the ground caustic sludge in a calcining kiln, calcining at 900-1200 ℃ for 40-60 minutes, cooling to obtain calcium oxide, selecting the calcium oxide, adding water for digestion, purifying, drying and sieving to obtain calcium hydroxide powder;
adding calcium hydroxide powder into 35% ammonium nitrate solution, mixing, heating in water bath, stirring, continuously supplementing evaporated water until ammonia smell is small, stopping heating, filtering, washing with water, and precipitating to obtain calcium nitrate tetrahydrate;
step four, further selecting the quartz sand tailings to enable the content of silicon dioxide to reach more than 99%;
and step five, mixing and stirring the calcium nitrate tetrahydrate, the carefully selected quartz sand tailings, the gypsum and the reinforcing agent to obtain the activating agent.
The principle of the invention is as follows:
the hardening of concrete is mainly carried out by means of the hydration process of cement, among which is the composition of portland cement clinker, tricalcium silicate (C)3S) 50-70%, dicalcium silicate (C)2S) accounts for 18-30 percent, and tricalcium aluminate (C)3A) 5-12% of tetracalcium aluminoferrite (C)4AF) accounts for 5 to 8 percent, wherein calcium silicate accounts for more than 70 percent. Tricalcium aluminate or dicalcium silicate is hydrated to generate calcium silicate hydrate (C-S-H) and Calcium Hydroxide (CH), the C-S-H is insoluble in water and immediately separated out as colloidal particles and gradually condensed into C-S-H gel, which is a source of cement material strength and guarantees the durability. CH is the main composition of the set cement, is an important composition for maintaining the alkalinity of the set cement, and is an important precondition for the stable existence of other set cement hydration products. In addition, tricalcium silicate is the early strength source of cement concrete, dicalcium silicate is the later strength source of cement concrete, and tricalcium silicate has a certain promotion effect on hydration of dicalcium silicate. The reaction equation of the hydration process of cement is as follows:
3CaO•SiO2+6H2O=3CaO•2SiO2•3H2o (colloid) +3Ca (OH)2(Crystal)
2(2CaO•SiO2)+4H2O=3CaO•2SiO2•3H2O+Ca(OH)2(Crystal)
3CaO•Al2O3+6H2O=3CaO•Al2O3•6H2O (Crystal)
Compared with the traditional method for exciting slag activity by adopting sulfate, the composite activator uses calcium nitrate, triethanolamine and nano silicon dioxide to replace a large amount of sulfate components, wherein the calcium salt component provides a large amount of calcium ions at the beginning of hydration, promotes CH to quickly reach saturation and quickly crystallize, and accelerates C together with gypsum3S, hydration of clinker; studies have shown that in cement concrete, NH4+Has early strength and coagulation promoting effect, and calcium nitrate can be used as early strength agent and antifreezing agent. The triethanolamine can quickly complex Al in liquid phase3+And, promoting C3S、C3A、C4AF and C3Early hydration of S, Al in liquid phase3+、Fe3+The combination of the plasma metal ions and the generation of a large amount of CH can accelerate the reaction rate of the slag; after the nano silicon dioxide is added, the filling effect and the volcanic ash activity of the nano silicon dioxide are utilized to promote the development of the early strength of the concrete. The composite activator promotes the development of the early strength of a cement-slag gelling system in all directions from multiple angles of accelerating the hydration of cement particles, CH generation and complexing of metal ions in a liquid phase to promote slag dissolution and reaction, optimizing particle accumulation, improving microstructure composition through secondary hydration of pozzolan active particles and the like, although the early excitation effect is still not as good as that of pure sodium sulfate, the risk of performance deterioration caused by the possibility of generation of a large amount of ettringite does not exist in the later period.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (7)
1. A high-content concrete activator is characterized in that: the composite material is prepared from the following raw materials in percentage by weight: 30-40% of alkaline residue, 15-25% of ammonium nitrate solution, 10-20% of quartz sand tailings, 10-20% of gypsum and 15-25% of reinforcing agent.
2. The high-content concrete activator according to claim 1, characterized in that: the composite material is prepared from the following raw materials in percentage by weight: 35% of alkaline residue, 25% of ammonium nitrate solution, 15% of quartz sand tailings, 10% of gypsum and 15% of reinforcing agent.
3. The high-content concrete activator according to claim 1, characterized in that: the main components and the weight percentage of the alkaline residue are as follows: 60-65% of calcium carbonate, 10-15% of calcium chloride and 15-28% of calcium hydroxide, wherein the particle size of the alkaline residue is not more than 75 μm, and the used alkaline residue is dechlorinated alkaline residue with the chlorine content of less than 0.3%.
4. The high-content concrete activator according to claim 1, characterized in that: the quartz sand tailings comprise the following main components in percentage by weight: 90-99% of silicon dioxide, and the particle size is not more than 75 μm.
5. The high-content concrete activator according to claim 1, characterized in that: the concentration of the sodium nitrate solution is 35%.
6. The high-content concrete activator according to claim 1, characterized in that: the reinforcing agent is triethanolamine.
7. A method for preparing the high-content concrete activator according to claim 1, which comprises the following steps: the method comprises the following steps:
grinding the dechlorinated alkaline residues, and controlling the particle size to be 40-80 mm;
placing the ground caustic sludge in a calcining kiln, calcining at 900-1200 ℃ for 40-60 minutes, cooling to obtain calcium oxide, selecting the calcium oxide, adding water for digestion, purifying, drying and sieving to obtain calcium hydroxide powder;
adding calcium hydroxide powder into 35% ammonium nitrate solution, mixing, heating in water bath, stirring, continuously supplementing evaporated water until ammonia smell is small, stopping heating, filtering, washing with water, and precipitating to obtain calcium nitrate tetrahydrate;
step four, further selecting the quartz sand tailings to enable the content of silicon dioxide to reach more than 99%;
and step five, mixing and stirring the calcium nitrate tetrahydrate, the carefully selected quartz sand tailings, the gypsum and the reinforcing agent to obtain the activating agent.
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Application publication date: 20200911 |