CN111848093A - Over-sulfur phosphogypsum phosphorus slag cement concrete product and preparation method thereof - Google Patents
Over-sulfur phosphogypsum phosphorus slag cement concrete product and preparation method thereof Download PDFInfo
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- CN111848093A CN111848093A CN202010815107.7A CN202010815107A CN111848093A CN 111848093 A CN111848093 A CN 111848093A CN 202010815107 A CN202010815107 A CN 202010815107A CN 111848093 A CN111848093 A CN 111848093A
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- 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
- 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
- C04B18/00—Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B18/04—Waste materials; Refuse
- C04B18/14—Waste materials; Refuse from metallurgical processes
- C04B18/141—Slags
- C04B18/145—Phosphorus slags
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Abstract
The invention discloses a sulfurous phosphogypsum phosphorus slag cement concrete product and a preparation method thereof, wherein the product comprises the following raw material components: phosphogypsum, phosphorous slag, silicate cement, sand, stones, a water reducing agent and water; according to the invention, through early-stage wet grinding of the phosphogypsum and the phosphorus slag, the strength of the material in each stage is greatly improved, the production process is simple, the cost is low, a large amount of industrial solid wastes can be used, and the environment protection is facilitated.
Description
Technical Field
The invention relates to a sulfurous phosphogypsum phosphorus slag cement concrete product and a preparation method thereof.
Background
Along with the rapid development of the society, the importance of environmental protection is increasingly highlighted, and the environmental protection needs to be done from all walks of life, and for the construction industry, the environment-friendly building and building materials are developed rapidly, and the construction of low-carbon cities is a necessary choice for the sustainable development of the society. Concrete is the most used building material at present, consuming nearly 40 billion cubic meters every year, wherein cement is one of the important materials constituting concrete, accounting for about 1/6 of the total amount of concrete. The cement production takes mineral resources as basic raw materials and fossil energy as main fuel, and is an industry mainly based on the operation mode of high energy consumption and high emission, such as a high-temperature kiln. Therefore, reducing the amount of the conventional portland cement used is one of the main solutions at present. The method for reducing the use amount of the cement mainly comprises two types, namely, the proportion of the cement in the concrete is reduced, namely, the proportion of mineral admixture or industrial waste residue in the cement concrete is improved, and a novel cementing material is developed.
Phosphogypsum is an industrial byproduct of phosphoric acid wet-process production of phosphorus chemical enterprises, and 5 tons of phosphogypsum are produced per 1 ton of phosphoric acid. Compared with other industrial by-product gypsums such as desulfurized gypsum, the phosphogypsum mainly has the disadvantages of strong acidity, and containing harmful elements such as phosphorus, fluorine and the like, thereby further influencing the scale and the utilization rate of the resource utilization of the phosphogypsum, and therefore, the resource utilization of the phosphogypsum is always a research hotspot of scholars at home and abroad; the phosphorus slag is an industrial byproduct in the process of preparing yellow phosphorus by an electric furnace method, the utilization degree of the phosphorus slag is not enough at present, the application field is narrow, the phosphorus slag is used as a cement mixed material, the early strength is not high due to the low early activity of the phosphorus slag, although various measures are adopted to improve the early strength of a phosphorus slag cement-based material at present, the overall strength improvement measure is not effective enough, and the application of large mixing amount of the phosphorus slag is not enough.
The phosphogypsum and the phosphorus slag are compounded to replace cement to prepare the over-sulfur phosphogypsum and phosphorus slag cement concrete product, so that the phosphogypsum can be recycled, and the large-dosage application of the phosphorus slag can be realized.
CN106747632A discloses a phosphorus slag, fly ash and phosphogypsum foam concrete, which is prepared from the following raw materials in percentage by weight: in the cementing material: 40-60% of cement, 20-40% of phosphorus slag powder, 10-30% of fly ash, 5-15% of the cementing material by using externally doped phosphogypsum as an activator, 0.6-1.2% of the cementing material by using a water reducing agent, 50-80% of a foaming agent and 0.2-0.3% of polypropylene fiber. CN109809786A discloses a phosphorous slag-based concrete and a preparation device thereof, wherein the concrete is composed of the following materials by mass: 20-40% of modified phosphorus slag powder, 10-20% of fly ash, 20-40% of cement, 5-15% of phosphogypsum, l-3% of additive and the balance of slag sand, wherein the additive is one or more of sodium aluminate, sodium sulfate and sodium silicate. In both inventions, the concrete utilizes the potential gelatinization of the phosphorus slag powder and the fly ash, the utilization rate of the phosphogypsum is lower, and the mixing amount of the cement is also higher.
Disclosure of Invention
Aiming at the defects of the prior art, the invention solves the problems that: provides a high-strength, low-cost and simple-process over-sulfur phosphogypsum phosphorus slag cement concrete product and a preparation method thereof.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
the over-sulfur phosphogypsum phosphorus slag cement concrete product comprises the following raw material components: phosphogypsum, phosphorous slag, silicate cement, sand, stones, a water reducing agent and water; the concrete comprises the following raw materials in parts by weight: 140-245 parts of phosphogypsum, 105-225 parts of phosphorous slag, 20-55 parts of silicate cement, 700-900 parts of sand, 1000-1100 parts of stones and 145-165 parts of water; the phosphogypsum, the phosphorus slag, the silicate cement and the water reducing agent jointly form a cementing material; the water reducing agent accounts for 0-0.5% of the weight of the cementing material.
Further, the concrete comprises the following raw materials in parts by weight: 170-215 parts of phosphogypsum, 135-195 parts of phosphorous slag, 24-45 parts of silicate cement, 1050-1070 parts of stones, 750-850 parts of sand, 155 parts of water and 0.2-0.4% of water reducing agent by mass of the cementing material.
Furthermore, the phosphogypsum is an industrial byproduct of wet-process phosphoric acid production of phosphorus chemical enterprises, and the main chemical component of the phosphogypsum is CaSO4·2H2O。
Further, the phosphorus slag is an industrial byproduct in the process of preparing yellow phosphorus by an electric furnace method; the main chemical components are as follows: silicon dioxide (SiO)2) Aluminum oxide (Al)2O3) Calcium oxide (CaO), magnesium oxide (MgO), phosphorus pentoxide (P)2O5)。
Further, the portland cement is portland cement, ordinary portland cement, portland slag, fly ash portland cement, pozzolanic portland cement, composite portland cement, or limestone portland cement; the main components are tricalcium silicate, dicalcium silicate, tricalcium aluminate, tetracalcium aluminoferrite, gypsum and a mixed material, and the strength grades are eight strength grades of 32.5, 32.5R, 42.5R, 52.5R, 62.5 and 62.5R.
Further, the water reducing agent is a BASF polycarboxylic acid type water reducing agent,
(II) any one or more of polycarboxylic acid high-efficiency water reducing agent, combined polycarboxylic acid water reducing agent and the like.
A preparation method of a sulfurous phosphogypsum phosphorus slag cement concrete product comprises the following steps:
s1, grinding phosphorous slag: adding water to wet-grind the phosphorous slag until the specific surface area is more than 280m2Obtaining phosphorus slag slurry with the solid content of 55-65% for later use;
s2, grinding phosphogypsum: adding 1-2% of ordinary portland cement into the phosphogypsum, adding water, and wet-grinding until the specific surface area is more than 350m2Obtaining phosphogypsum slurry with the solid content of 55-65% for later use;
s3, filtering and concentrating: filtering and concentrating the phosphorus slag slurry and the phosphogypsum slurry with the solid content of 55-65% to obtain phosphorus slag mud and phosphogypsum mud with the solid content of 75-85% for later use;
s4, mixing and stirring: adding water into the phosphogypsum mud, the phosphorus slag mud, the ordinary portland cement, the stones, the sand and the water reducing agent together, fully mixing and uniformly stirring to obtain the over-sulfur phosphogypsum phosphorus slag cement concrete, and then pressing or pouring to obtain a product;
s5, product maintenance: after the over-sulfur phosphogypsum phosphorus slag cement concrete product is molded, standing for 0-1 day, slowly heating to 50-75 ℃ from the normal temperature, steaming at the temperature for 1-3 days, taking out, soaking in water for 0-1 day, and sealing and packaging with plastic cloth for delivery.
The invention has the advantages of
The phosphogypsum is used as a matrix material of the over-sulfur phosphogypsum phosphorus slag cement concrete product, the mixing amount is large, harmful impurities in the phosphogypsum greatly delay the hydration of a gelling component, which is a main reason for overlong setting time and low early strength. Firstly, in the phosphogypsum wet-grinding modification process, cement is hydrated to generate calcium hydroxide and the like, the calcium hydroxide and the like react with phosphorus and fluorine impurities in phosphogypsum to generate inert substances, and the weakening effect of the phosphorus and fluorine impurities on intermolecular force of a cementing material is eliminated, so that the setting time is shortened, and the strength of a high-sulfur phosphogypsum phosphorus slag cement concrete product can be improved; secondly, the phosphogypsum wet grinding modification converts the acidic phosphogypsum into alkalinity, the alkalinity required by phosphorus slag hydration can be met in a short time, and the external condition of phosphorus slag hydration is effectively provided; in addition, a small amount of cement is doped to form a small amount of hydration product crystal nuclei in the phosphogypsum slurry, the hydration product crystal nuclei are uniformly distributed in the phosphogypsum slurry through wet grinding, and after phosphorous slag and cement are added in the process of preparing the sulfur-passing phosphogypsum phosphorous slag cement concrete product, the hydration product grows around the crystal nuclei, so that microcracks are blocked, hardened body pores are filled, the density of a hardened body is increased, and the strength of the sulfur-passing phosphogypsum phosphorous slag cement concrete product is finally improved.
Detailed Description
The present invention will be described in further detail below.
A preparation method of a sulfurous phosphogypsum phosphorus slag cement concrete product comprises the following steps:
s1, grinding phosphorous slag: adding water to the phosphorous slag for wet grinding until the specific surface area is 481.2m2And/kg, obtaining phosphorus slag slurry with the solid content of 57.3 percent for later use.
S2, grinding phosphogypsum: adding 1 percent of ordinary portland cement into the phosphogypsum, adding water, and wet-grinding to the specific surface area of 413.5m2And/kg, obtaining phosphogypsum slurry with the solid content of 57.5 percent for later use.
S3, filtering and concentrating: and filtering and concentrating the phosphorus slag slurry and the phosphogypsum slurry to obtain phosphorus slag mud with the solid content of 78.2 percent and phosphorus gypsum mud with the solid content of 77.6 percent for later use.
S4, mixing and stirring: the method comprises the steps of adding water into phosphogypsum mud, phosphorus slag mud, ordinary portland cement, stones, sand and a water reducing agent together, fully mixing and uniformly stirring to obtain the over-sulfur phosphogypsum phosphorus slag cement concrete, and then pressing or pouring to obtain a product.
S5, product maintenance: after the over-sulfur phosphogypsum phosphorus slag cement concrete product is formed, standing for 1 day, slowly heating to 75 ℃ from the normal temperature, steaming at the temperature for 1 day, taking out, soaking in water for 1 day, and sealing and packaging by using plastic cloth for delivery.
The concrete proportion and test results of the 10L of over-sulfur phosphogypsum phosphorus slag cement concrete prepared by the method are shown in the following table.
The over-sulfur phosphogypsum phosphorus slag cement concrete prepared by the method can generate a series of hydration reactions, namely has hydraulicity. In the concrete, sand and stones play a role of a skeleton, and phosphogypsum, phosphorous slag, silicate cement and a water reducing agent jointly form a cementing material and play a role of cementing sand and stone. Experiments show that a large amount of needle-shaped hydrated calcium sulphoaluminate and amorphous hydrated calcium silicate minerals are formed on the surfaces of phosphogypsum particles and among the particles, so that higher strength is generated, and the phosphogypsum plays a role of a cementing material; in the cementing material, a part of phosphogypsum plays a role of a skeleton (the amount of the phosphogypsum of the invention is remained relative to the phosphorus slag and silicate cement, namely, the part of phosphogypsum is not completely reacted), and a part of phosphogypsum participates in a chemical reaction to form a series of new hydration products. The over-sulfur phosphogypsum phosphorus slag cement concrete prepared by the method has qualified stability and quite high strength, can be prepared into C20, C25 and C30 grades, and is suitable for being used as general building materials, wall materials and road materials.
In the invention, 0-2% of silicate cement is added into the phosphogypsum, so that acidic substances in the phosphogypsum are neutralized, and the early strength of the over-sulfur phosphogypsum phosphorus slag cement concrete prepared from the phosphogypsum is improved.
The phosphogypsum is used as a matrix material of the over-sulfur phosphogypsum phosphorus slag cement concrete product, so that the doping amount of the phosphogypsum is large, and harmful impurities in the phosphogypsum greatly delay the hydration of a gelling component, which is a main reason for overlong setting time and low early strength. Firstly, in the phosphogypsum wet-grinding modification process, cement is hydrated to generate calcium hydroxide and the like, the calcium hydroxide and the like react with phosphorus and fluorine impurities in the phosphogypsum to generate inert substances, and the weakening effect of the phosphorus and fluorine impurities on intermolecular force of a cementing material is eliminated, so that the setting time is shortened, and the strength of a high-sulfur phosphogypsum phosphorus slag cement concrete product can be improved. And secondly, the phosphogypsum wet grinding modification converts the acidic phosphogypsum into alkalinity, so that the alkalinity required by phosphorus slag hydration can be met in a short time, and the external condition of phosphorus slag hydration is effectively provided. In addition, a small amount of cement is doped to form a small amount of hydration product crystal nuclei in the phosphogypsum slurry, the hydration product crystal nuclei are uniformly distributed in the phosphogypsum slurry through wet grinding, and after phosphorous slag and cement are added in the process of preparing the sulfur-passing phosphogypsum phosphorous slag cement concrete product, the hydration product grows around the crystal nuclei, so that microcracks are blocked, hardened body pores are filled, the density of a hardened body is increased, and the strength of the sulfur-passing phosphogypsum phosphorous slag cement concrete product is finally improved.
The wet grinding process of the phosphorous slag provided by the invention promotes the dissolution of silicon, calcium and aluminum in the phosphorous slag, depolymerizes the glass phase structure of the phosphorous slag under the action of mechanical force and releases active SiO2And Al2O3Cement added in the preparation process provides an alkaline environment for hydration of the cementing material, and phosphogypsum provides SO4 2-The conditions are created for further hydrolysis of the phosphorus slag, ettringite and C-S-H gel are generated by reaction, and the periphery of unreacted phosphogypsum is wrapped by various compact hydration products along with the increase of age to play a role of filling the micro-aggregate; in the over-sulfur phosphogypsum phosphorus slag cement concrete cementing material system, because the phosphogypsum is doped in a large amount, gypsum is always hydrated in the hydration processAre surplus, so that the formation of ettringite is somewhat dependent on Ca (OH) during hydration2Content and Al3+Controlled content of Ca (OH)2The content depends on the amount of the silicate cement and the hydration rate of the silicate cement, Al3+The content depends on the hydrolysis speed of the phosphorous slag, and the alkalinity of the liquid phase greatly affects the hydrolysis speed of the phosphorous slag, so the amount of the silicate cement directly affects the quantity of the ettringite, when the amount of the silicate cement is low, hydration products formed by the hydration of the silicate cement are less, the alkalinity of the liquid phase is low, the hydration activity of the phosphorous slag can not be fully excited, the slurry structure is loose, and the macroscopic expression shows that the strength is low. When the amount of the silicate cement is excessive, although the silicate cement hydrates to form more hydration products and provides a sufficient alkaline environment for phosphorus slag hydration, excessive ettringite is continuously formed in the hardened slurry to cause volume expansion, so that the structure of the slurry is damaged, the compactness of the slurry is reduced, and the strength is reduced, therefore, the amount of the silicate cement must be proper. Meanwhile, the curing method provided by the invention is more beneficial to the development of the strength of the over-sulfur phosphogypsum phosphorus slag cement concrete product.
The invention has the following main characteristics:
1) the prepared over-sulfur phosphogypsum phosphorus slag cement concrete has the characteristic of hydraulicity.
2) The prepared over-sulfur phosphogypsum phosphorus slag cement concrete has certain early strength and quite high later strength, and has the characteristics of good workability, convenient construction and forming and the like.
3) The main raw materials are industrial waste residues such as phosphogypsum and phosphorus slag, the production process is simple, the cost is low, energy can be saved, and a large amount of carbon dioxide can be prevented from being discharged; but also can use a large amount of industrial waste residues, change waste into valuable, is beneficial to energy conservation, consumption reduction and environmental protection, and obviously reduces the manufacturing cost of buildings or concrete products.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. The over-sulfur phosphogypsum phosphorus slag cement concrete product is characterized by comprising the following raw material components: phosphogypsum, phosphorous slag, silicate cement, sand, stones, a water reducing agent and water; the concrete comprises the following raw materials in parts by weight: 140-245 parts of phosphogypsum, 105-225 parts of phosphorous slag, 20-55 parts of silicate cement, 700-900 parts of sand, 1000-1100 parts of stones and 145-165 parts of water; the phosphogypsum, the phosphorus slag, the silicate cement and the water reducing agent jointly form a cementing material; the water reducing agent accounts for 0-0.5% of the weight of the cementing material.
2. The over-sulfur phosphogypsum phosphorus slag cement concrete product according to claim 1, which is characterized in that the raw materials in parts by weight of the concrete per side are as follows: 170-215 parts of phosphogypsum, 135-195 parts of phosphorous slag, 24-45 parts of silicate cement, 1050-1070 parts of stones, 750-850 parts of sand, 155 parts of water and 0.2-0.4% of water reducing agent by mass of the cementing material.
3. The over-sulfur phosphogypsum phosphorus slag cement concrete product according to claim 1, which is an industrial byproduct of phosphoric acid wet production by phosphorus chemical enterprises.
4. The resulfurized phosphogypsum phosphorus slag cement concrete product according to claim 1, characterized in that the phosphorus slag is an industrial by-product in the preparation of yellow phosphorus by electric furnace process.
5. The resulfurized phosphogypsum phosphorus slag cement concrete product according to claim 1, characterized in that the portland cement is portland cement, ordinary portland cement, slag silicate, fly ash portland cement, pozzolanic portland cement, composite portland cement or limestone portland cement.
6. According to the rightThe over-sulfur phosphogypsum phosphorus slag cement concrete product of claim 1, which is characterized in that the water reducing agent is a BASF polycarboxylic acid type water reducing agent,
(II) any one or more of polycarboxylic acid high-efficiency water reducing agent, combined polycarboxylic acid water reducing agent and the like.
7. A preparation method of a over-sulfur phosphogypsum phosphorus slag cement concrete product is characterized by comprising the following steps:
s1, grinding phosphorous slag: adding water to wet-grind the phosphorous slag until the specific surface area is more than 280m2Obtaining phosphorus slag slurry with the solid content of 55-65% for later use;
s2, grinding phosphogypsum: adding 1-2% of ordinary portland cement into the phosphogypsum, adding water, and wet-grinding until the specific surface area is more than 350m2Obtaining phosphogypsum slurry with the solid content of 55-65% for later use;
s3, filtering and concentrating: filtering and concentrating the phosphorus slag slurry and the phosphogypsum slurry with the solid content of 55-65% to obtain phosphorus slag mud and phosphogypsum mud with the solid content of 75-85% for later use;
s4, mixing and stirring: adding water into the phosphogypsum mud, the phosphorus slag mud, the ordinary portland cement, the stones, the sand and the water reducing agent together, fully mixing and uniformly stirring to obtain the over-sulfur phosphogypsum phosphorus slag cement concrete, and then pressing or pouring to obtain a product;
s5, product maintenance: after the over-sulfur phosphogypsum phosphorus slag cement concrete product is molded, standing for 0-1 day, slowly heating to 50-75 ℃ from the normal temperature, steaming at the temperature for 1-3 days, taking out, soaking in water for 0-1 day, and sealing and packaging with plastic cloth for delivery.
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| CN115259729A (en) * | 2022-08-19 | 2022-11-01 | 湖北昌耀新材料工程技术研究有限责任公司 | Excessive-sulfur phosphogypsum-slag cementing material modifier, application thereof and excessive-sulfur phosphogypsum-slag cementing material composition |
| US11912630B2 (en) * | 2022-05-30 | 2024-02-27 | Hubei University Of Technology | Method of preparing recycled cementitious material by phosphogypsum-assisted carbon sequestration pretreatment process |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113735545A (en) * | 2021-10-21 | 2021-12-03 | 江苏一夫科技股份有限公司 | Concrete product containing phosphogypsum fly ash cement and preparation method thereof |
| US11912630B2 (en) * | 2022-05-30 | 2024-02-27 | Hubei University Of Technology | Method of preparing recycled cementitious material by phosphogypsum-assisted carbon sequestration pretreatment process |
| CN115259729A (en) * | 2022-08-19 | 2022-11-01 | 湖北昌耀新材料工程技术研究有限责任公司 | Excessive-sulfur phosphogypsum-slag cementing material modifier, application thereof and excessive-sulfur phosphogypsum-slag cementing material composition |
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Application publication date: 20201030 |