CN114133201A - Multi-scale solid waste modified phosphorus building gypsum composite cementing material - Google Patents
Multi-scale solid waste modified phosphorus building gypsum composite cementing material Download PDFInfo
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- CN114133201A CN114133201A CN202111644895.9A CN202111644895A CN114133201A CN 114133201 A CN114133201 A CN 114133201A CN 202111644895 A CN202111644895 A CN 202111644895A CN 114133201 A CN114133201 A CN 114133201A
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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
- 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
- C04B28/14—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 calcium sulfate cements
- C04B28/142—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 calcium sulfate cements containing synthetic or waste calcium sulfate cements
- C04B28/143—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 calcium sulfate cements containing synthetic or waste calcium sulfate cements the synthetic calcium sulfate being phosphogypsum
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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
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
Abstract
The invention provides a multi-scale solid waste modified phosphorus building gypsum composite cementing material which comprises the following raw materials in parts by weight: 60-70 parts of phosphorus building gypsum, 2-5 parts of carbide slag, 5-15 parts of steel slag, 10-25 parts of blast furnace nickel slag, 5-10 parts of superfine slag, 0-0.1 part of retarder, 0.2-0.4 part of water reducer and 0-0.05 part of water-retaining agent. The phosphorus building gypsum is used as a main raw material, and acetylene sludge, steel slag, blast furnace nickel slag and superfine slag are doped to modify the phosphorus building gypsum, and the alkaline action of solid waste is utilized to react with soluble phosphorus, fluorine and other impurities in the phosphogypsum to generate insoluble precipitate so as to solidify harmful impurities in the phosphogypsum; the composite cementing material for the phosphorus building gypsum has excellent mechanical property and water resistance while realizing the cooperative treatment and resource utilization of various solid wastes, and provides a rubber material system with excellent performance for the large-scale resource utilization of the phosphogypsum.
Description
Technical Field
The invention belongs to the technical field of building materials, and relates to a multi-scale solid waste modified phosphorus building gypsum composite cementing material.
Background
Phosphogypsum is a solid waste produced in a wet-process phosphoric acid process, and the components of the phosphogypsum are mainly calcium sulfate dihydrate. For every 1 ton of phosphoric acid produced, 4.5-5 tons of phosphogypsum are produced. Because the phosphogypsum contains harmful impurities such as phosphorus, fluorine, organic matters, heavy metals, radioactivity and the like, and the influence caused by the impurities is eliminated by lacking an effective pretreatment technology at present, products prepared by taking the phosphogypsum as a raw material are rare. At the present stage, the utilization rate of the phosphogypsum in China is less than 10%, the stacking and releasing amount of the phosphogypsum is increased year by year, and more than 7000 million tons of phosphogypsum are newly increased in recent years, so that a large amount of land resources are occupied, serious environmental problems are caused, and the balance of human health and an ecological system is finally damaged. Based on the above, it is a technical problem to be solved urgently to research and develop a method capable of effectively utilizing the phosphogypsum, and improve the utilization rate of solid waste materials, so as to realize the recycling of resources and the protection of the environment.
Chinese patent CN202010896686.2 discloses a method for preparing pure calcium sulfate whisker from carbide slag modified phosphogypsum. The feed is prepared from the following raw materials: the mass ratio of the phosphogypsum powder to the carbide slag powder is 100:5-25, the mass ratio of the organic solvent to the water is 1:1, the weight percentage of the retarder is 0.1-0.3, and the weight percentage of the water reducing agent is 0.1-0.5. The method fully utilizes phosphorus solid waste and carbide slag to prepare the anhydrous calcium sulfate whisker at room temperature, combines a wet grinding process to dissolve out impurities of the phosphogypsum and the carbide slag, removes the impurities by utilizing organic matters and water, obtains the calcium sulfate with higher purity through simple lengthening and crystal growth, and further prepares the anhydrous calcium sulfate whisker. However, the above patent has a problem that the admixture added is too single, resulting in low hydration activity, low strength of the product and the like.
Chinese patent CN202010530908.9 discloses a high-strength water-resistant phosphogypsum composite cementing material and a preparation method thereof, wherein industrial solid wastes such as solid sulfur ash, gasified slag and the like are modified to prepare the environment-friendly, low-cost and high-strength water-resistant phosphogypsum composite cementing material. However, the sulfur content in the sulfur-fixing ash used in the above patent is high (in terms of SO)310 percent), and the volume stability is poor, thereby limiting the resource utilization of the building materials.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a multi-scale solid waste modified phosphorus building gypsum composite cementing material, which takes phosphorus building gypsum as a main raw material and is matched with various solid waste raw materials with different scales to modify phosphogypsum, and has the advantages of high mechanical strength, good water resistance and the like.
In order to solve the technical problems, the invention adopts the following technical scheme: the multi-scale solid waste modified phosphorus building gypsum composite cementing material comprises the following raw materials in parts by weight:
60-70 parts of phosphorus building gypsum, 2-5 parts of carbide slag, 5-15 parts of steel slag, 10-25 parts of blast furnace nickel slag, 5-10 parts of superfine slag, 0-0.1 part of retarder, 0.2-0.4 part of water reducer and 0-0.05 part of water-retaining agent; the superfine slag is prepared by wet grinding granulated blast furnace slag, and the particle size of the superfine slag is 0.5-2 mu m.
In the invention, phosphorus building gypsum is used as a main raw material, and four solid waste raw materials of carbide slag, steel slag, blast furnace nickel slag and superfine slag are used as admixture, wherein the carbide slag in the raw materials mainly comprises calcium hydroxide and calcium oxide, and the calcium hydroxide and the calcium oxide account for about 70 percent; the content of calcium oxide in the steel slag is 40-60%, and strong alkaline calcium hydroxide can be generated when the steel slag meets water, so that a solution environment capable of fully playing an alkaline role is provided. The blast furnace nickel slag in the raw materials has a large amount of vitreous bodies, and has certain gelling property after being crushed; in addition, the nickel slag has a porous surface and can be combined with other powder materials, so that the preparation cost is obviously reduced.
The phosphorous building gypsum composite cementing material is prepared from the raw materials in parts by weight, and the acetylene sludge, the steel slag, the blast furnace nickel slag and the superfine slag can fully exert the synergistic modification effect on the phosphorous building gypsum: on one hand, based on the particle size difference of different types of solid waste admixtures, especially the superfine slag with the particle size of 0.5-2 mu m processed by adopting a wet grinding technology has the effects of micro-aggregate and dense filling while improving the hydration activity of solid waste, thereby improving the strength and the water resistance of the product; on the other hand, the alkaline environment provided by various solid wastes not only can neutralize the impurities such as soluble phosphorus, fluorine and the like in the phosphogypsum to play a role of solidifying the impurities, but also can excite other low-activity admixtures to generate hydration reaction with gypsum to generate hydration products such as C-S-H gel, ettringite and the like for enhancing the strength and durability of the system, thereby further improving the mechanical property of the product. Researches find that when four solid waste admixtures are used together, compared with the use of only 1-3 of the admixtures, the modification effect is better, and the mechanical property and the water resistance of the final product are better.
Preferably, the superfine slag is prepared by wet grinding granulated blast furnace slag according to a water-solid ratio (mass ratio) of 0.5-0.8, the water-solid ratio is limited within the range of 0.5-0.8, the wet grinding is carried out on the basis of ensuring the fluidity of the superfine slag to be 180mm +/-5 mm, the particle size of the obtained superfine slag is 0.5-2 mu m, and the median particle size is smaller than 2 mu m, so that the micro-aggregate effect of the cementing material can be better exerted, fine pores are filled, and the structure is more compact.
Further, the phosphorus building gypsum is obtained by calcining dihydrate gypsum at the temperature of 130-150 ℃, and has the rupture strength of more than 2.5MPa in 2h and the absolute dry compressive strength of more than 9.5 MPa.
Further, the carbide slag is obtained by drying and grinding waste slag generated in acetylene preparation and sieving the waste slag through a 90-micrometer square-hole sieve, and the residue on the sieve is not more than 15%.
Further, the steel slag is a byproduct of steel-making production, wherein the content of calcium oxide is 40-60%, and the specific surface area is 600-800 m2/kg。
Further, the blast furnace nickel slag is obtained by drying and grinding solid waste slag generated in the process of smelting ferronickel alloy and then sieving the solid waste slag through a 80-micrometer square-hole sieve, wherein the residue on sieve is not more than 5%.
Further, the retarder is selected from gypsum special retarder and/or citric acid retarder.
Further, the water reducing agent is selected from a polycarboxylate water reducing agent and/or a melamine water reducing agent, and the water reducing rate of the water reducing agent is more than 15%.
Further, the water-retaining agent is hydroxypropyl methyl cellulose ether, and the viscosity of the water-retaining agent is 500-10000 mPa & s.
On the basis of the technical scheme, the particle size of the phosphorus building gypsum is 3-32 mu m; the particle size of the carbide slag is 10-40 mu m; the particle size of the steel slag is 1-10 mu m; the particle size of the blast furnace nickel slag is 50-80 μm. The raw materials with different particle sizes can be obtained by crushing and pretreating the raw materials by a crusher.
The method comprises the steps of pretreating solid waste raw materials to obtain four solid waste admixtures with different particle size gradients including superfine slag, and matching the admixtures with different particle sizes with the phosphorus building gypsum to give full play to the collective and matching effect of various admixtures structurally, so that pores in the gypsum are effectively filled, the structure is densely filled, and the strength and the water resistance are improved; functionally, various solid waste raw materials play a role in synergistic modification, fully play the roles of hydration activity and alkaline excitation, further improve the comprehensive performance and realize the efficient utilization of various solid wastes.
Further, the multi-scale solid waste modified phosphorus building gypsum composite cementing material can be prepared by adopting the following method: weighing the following raw materials in parts by weight: phosphorus building gypsum, carbide slag, steel slag, blast furnace nickel slag, superfine slag, a retarder, a water reducing agent and a water-retaining agent; and (3) uniformly mixing water and the raw materials according to a water-material ratio (mass ratio) of 0.4-0.6 to obtain the multi-scale solid waste modified phosphorus building gypsum composite cementing material.
In summary, the invention utilizes various solid wastes to modify the phosphorus building gypsum, on one hand, the alkaline action of the solid wastes can react with the soluble phosphorus, fluorine and other impurities in the phosphogypsum to generate insoluble precipitate, thereby playing the role of solidifying harmful impurities; on the other hand, the construction of the alkaline solution environment can better stimulate the hydration activity of solid wastes such as steel slag, blast furnace nickel slag and the like, and can generate hydration reaction with gypsum to generate hydration products such as water-resistant C-S-H gel, ettringite and the like, thereby increasing the mechanical strength and the water resistance of the system. In addition, the superfine slurry-like slag admixture prepared by wet grinding is introduced, so that the dissolution of active ions such as calcium, silicon, aluminum and the like in various solid wastes can be promoted, the hydration activity of the solid wastes can be improved, the generation of water-resistant hydration products is promoted, the early strength of a system is improved, the micro-aggregate effect of a cementing material can be fully exerted, gaps are filled, and the durability of hardened slurry is improved.
Compared with the prior art, the invention has the beneficial effects that:
(1) the phosphorus building gypsum composite cementing material provided by the invention takes phosphorus building gypsum as a main raw material (the dosage of the phosphorus building gypsum in the raw material is 60-70 wt%), acetylene sludge, steel slag, blast furnace nickel slag and superfine slag are added to modify the phosphorus building gypsum, and the alkaline action of various solid wastes can react with soluble phosphorus, fluorine and other impurities in phosphogypsum to generate insoluble precipitates, so that the effect of solidifying harmful impurities is achieved. Through hydration activation and particle effect of the solid wastes with different scales, the utilization rate of various solid wastes is effectively improved, and the cooperative treatment and resource utilization of the phosphorus building gypsum and various solid wastes are realized.
(2) The phosphorus building gypsum composite cementing material provided by the invention has the 1d compressive strength of 6.6-7.4 MPa, the 7d compressive strength of 10.6-11.5 MPa, the 28d compressive strength of 15.1-16.2 MPa, the 28d absolute dry compressive strength of 23.5-24.9 MPa and the softening coefficient of 0.68-0.74, has excellent mechanical properties and water resistance, and provides an excellent-performance cementing material system for large-scale resource utilization of phosphogypsum.
Drawings
FIG. 1 is a schematic diagram of the mechanical properties of the phosphorus building gypsum composite cementitious material provided in examples 1 to 5 of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention.
The weight parts of the raw materials involved in the embodiments 1-5 of the invention are shown in the following table 1:
TABLE 1
In the above table 1, the phosphorous building gypsum is obtained by calcining dihydrate gypsum at 130-150 ℃, the rupture strength of 2h is more than 2.5MPa, the absolute dry compressive strength is more than 9.5MPa, and CaSO in the phosphorous building gypsum4·0.5H2The mass fraction of O is more than 85 percent; the used carbide slag is obtained by drying and grinding waste slag generated in acetylene preparation and sieving the waste slag through a 90-micrometer square-hole sieve, and the residue on the sieve is not more than 15 percent; used ofThe steel slag is a byproduct in steel-making production, wherein the content of calcium oxide is 40-60%, and the specific surface area is 600-800 m2Per kg; the used blast furnace nickel slag is obtained by drying, grinding and sieving solid waste slag generated in the process of smelting ferronickel alloy, and the residue of the solid waste slag is not more than 5 percent through a 80-micron square-hole sieve; the retarder is one or two of special gypsum retarder and citric acid retarder mixed according to any proportion; the water reducing agent is one of a polycarboxylic acid water reducing agent and a melamine water reducing agent, and the water reducing rate is more than 15%; the water-retaining agent is hydroxypropyl methyl cellulose ether, and the viscosity is 500-10000 mPa & s; the superfine slag is prepared by wet grinding granulated blast furnace slag, and the particle size of the superfine slag is 0.5-2 mu m.
Example 1
Weighing the following raw materials in parts by weight as shown in Table 1: phosphorus building gypsum, carbide slag, steel slag, blast furnace nickel slag, superfine slag, a retarder, a water reducing agent and a water-retaining agent;
and (3) mixing water and the raw materials according to the water-material ratio (mass ratio) of 0.40, and uniformly stirring to obtain the phosphorus building gypsum composite cementing material.
Example 2
Weighing the following raw materials in parts by weight as shown in Table 1: phosphorus building gypsum, carbide slag, steel slag, blast furnace nickel slag, superfine slag, a retarder, a water reducing agent and a water-retaining agent;
and mixing water and the raw materials according to the water-material ratio (mass ratio) of 0.45, and uniformly stirring to obtain the phosphorus building gypsum composite cementing material.
Example 3
Weighing the following raw materials in parts by weight as shown in Table 1: phosphorus building gypsum, carbide slag, steel slag, blast furnace nickel slag, superfine slag, a retarder, a water reducing agent and a water-retaining agent;
and mixing water and the raw materials according to the water-material ratio (mass ratio) of 0.52, and uniformly stirring to obtain the phosphorus building gypsum composite cementing material.
Example 4
Weighing the following raw materials in parts by weight as shown in Table 1: phosphorus building gypsum, carbide slag, steel slag, blast furnace nickel slag, superfine slag, a retarder, a water reducing agent and a water-retaining agent;
and (3) mixing water and the raw materials according to the water-material ratio (mass ratio) of 0.56, and uniformly stirring to obtain the phosphorus building gypsum composite cementing material.
Example 5
Weighing the following raw materials in parts by weight as shown in Table 1: phosphorus building gypsum, carbide slag, steel slag, blast furnace nickel slag, superfine slag, a retarder, a water reducing agent and a water-retaining agent;
and mixing water and the raw materials according to the water-material ratio (mass ratio) of 0.60, and uniformly stirring to obtain the phosphorus building gypsum composite cementing material.
Comparative example
This comparative example is substantially the same as example 1 except that the ultrafine slag in example 1 was replaced with an equal part by weight of ordinary slag which was not subjected to wet grinding.
Application example
Performance testing was performed on the phosphorous building gypsum composite cementitious materials prepared in examples 1-5 and comparative examples, involving a test method comprising: and testing the compression strength and the softening coefficient of the gypsum. Wherein, the gypsum compression strength test is according to the national standard: the operation is carried out according to the requirements of the determination of the mechanical property of the building gypsum (GB/T9776-. The softening coefficient test was conducted according to the requirements of the building materials industry Standard (JC/T698-1998).
The results of the relevant tests are shown in table 2 below:
TABLE 2
As can be seen from the above table,
the comparative example uses ordinary slag as a raw material without wet grinding treatment, in which the median particle diameter is large and it is difficult to achieve filling of fine voids. Compared with example 1, the phosphorus building gypsum composite cementing material prepared by the comparative example not only has lower mechanical strength, but also has less ideal water resistance.
In the embodiments 1-5 of the invention, the superfine slag obtained by wet grinding is used as a raw material, and the mechanical property and the water resistance of the product are obviously improved compared with those of a comparative example. Wherein the 1d compressive strength is 6.6-7.4 MPa, the 7d compressive strength is 10.6-11.5 MPa, the 28d compressive strength is 15.1-16.2 MPa, the 28d absolute dry compressive strength is 23.5-24.9 MPa, and the softening coefficient is 0.68-0.74. The invention adopts a wet grinding method to treat the slag raw material, can reduce the median particle size of the slag raw material, fully exerts the micro-aggregate effect of the cementing material, can fill fine pores to ensure that the product structure is more compact, promotes the dissolution of active ions such as calcium, silicon, aluminum and the like in the slag in the wet grinding process, improves the hydration activity of solid waste, generates hydration products such as C-S-H gel, ettringite and the like, and further improves the mechanical strength and the water resistance of the product.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (10)
1. The multi-scale solid waste modified phosphorus building gypsum composite cementing material is characterized by comprising the following raw materials in parts by weight: 60-70 parts of phosphorus building gypsum, 2-5 parts of carbide slag, 5-15 parts of steel slag, 10-25 parts of blast furnace nickel slag, 5-10 parts of superfine slag, 0-0.1 part of retarder, 0.2-0.4 part of water reducer and 0-0.05 part of water-retaining agent; the superfine slag is prepared by wet grinding granulated blast furnace slag, and the particle size of the superfine slag is 0.5-2 mu m.
2. The multi-scale solid waste modified phosphorus building gypsum composite cementitious material as claimed in claim 1, wherein in the wet grinding, the mass ratio of water to the granulated blast furnace slag is 0.5-0.8: 1.
3. the multi-scale solid waste modified phosphorus building gypsum composite cementing material according to claim 1, wherein the phosphorus building gypsum is obtained by calcining dihydrate gypsum at 130-150 ℃, and the 2h flexural strength of the phosphorus building gypsum composite cementing material is more than 2.5MPa, and the absolute dry compressive strength of the phosphorus building gypsum composite cementing material is more than 9.5 MPa.
4. The multi-scale solid waste modified phosphorus building gypsum composite cementing material according to claim 1, wherein the carbide slag is obtained by drying, grinding and sieving waste slag generated in acetylene preparation, the sieving adopts a square hole sieve with the aperture of 90 μm, and the residue of the sieving is not more than 15%.
5. The multi-scale solid waste modified phosphorus building gypsum composite cementing material as claimed in claim 1, wherein the steel slag is a byproduct of steel-making production, the calcium oxide content of the steel slag is 40-60%, and the specific surface area of the steel slag is 600-800 m2/kg。
6. The multi-scale solid waste modified phosphorus building gypsum composite cementing material of claim 1, wherein the blast furnace nickel slag is obtained by drying, grinding and sieving solid waste slag generated in the process of smelting ferronickel alloy, the sieving adopts a square hole sieve with the pore diameter of 80 μm, and the residue of the sieving is not more than 5%.
7. The multi-scale solid waste modified phosphorous building gypsum composite cementitious material of claim 1, wherein the set retarder is selected from gypsum specific set retarders and/or citric acid type set retarders.
8. The multi-scale solid waste modified phosphorus building gypsum composite cementitious material of claim 1, wherein the water reducing agent is selected from a polycarboxylate water reducing agent and/or a melamine water reducing agent, and the water reducing rate of the water reducing agent is more than 15%.
9. The multiscale solid waste modified phosphorus building gypsum composite cementitious material of claim 1, characterised in that the water retention agent is hydroxypropyl methyl cellulose ether with a viscosity of 500 to 10000 mPa-s.
10. The multi-scale solid waste modified phosphorus building gypsum composite cementing material as claimed in claim 1, wherein the particle size of the phosphorus building gypsum is 3-32 μm, the particle size of the carbide slag is 10-40 μm, the particle size of the steel slag is 1-10 μm, and the particle size of the blast furnace nickel slag is 50-80 μm.
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| CN114804915A (en) * | 2022-05-27 | 2022-07-29 | 湖北工业大学 | Multifunctional light building material and preparation method and application thereof |
| CN115849853A (en) * | 2022-12-16 | 2023-03-28 | 长沙矿山研究院有限责任公司 | Large-doped-amount fluorgypsum-based multielement solid waste filling cementing material and preparation method thereof |
| CN115947582A (en) * | 2022-07-21 | 2023-04-11 | 湖北工业大学 | Cementitious material and uses thereof |
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