GB2607658A - Method for preparing calcium sulphosilicate-dicalcium silicate-calcium sulphoaluminate system from calcium carbide slag and method for improving late-stage - Google Patents

Method for preparing calcium sulphosilicate-dicalcium silicate-calcium sulphoaluminate system from calcium carbide slag and method for improving late-stage Download PDF

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GB2607658A
GB2607658A GB2203020.9A GB202203020A GB2607658A GB 2607658 A GB2607658 A GB 2607658A GB 202203020 A GB202203020 A GB 202203020A GB 2607658 A GB2607658 A GB 2607658A
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calcium
sulphosilicate
carbide slag
cement
raw meal
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GB202203020D0 (en
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Cui Suping
Xu Lulu
Wang Yali
Lan Mingzhang
Wang Jianfeng
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Beijing University of Technology
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Beijing University of Technology
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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
    • C04B7/00—Hydraulic cements
    • C04B7/32—Aluminous cements
    • C04B7/323—Calcium aluminosulfate cements, e.g. cements hydrating into ettringite
    • 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
    • C04B40/0046—Premixtures of ingredients characterised by their processing, e.g. sequence of mixing the ingredients when preparing the premixtures
    • 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
    • C04B7/00—Hydraulic cements
    • C04B7/14—Cements containing slag
    • 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
    • C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
    • C04B22/0006—Waste inorganic materials
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)

Abstract

A method for preparing a calcium sulphosilicate-dicalcium silicate-calcium  sulphoaluminate system from a calcium carbide slag is disclosed which comprises preparation of raw meal by grinding calcium carbide slag, silica fume, and one of  phosphogypsum and desulfurized gypsum by a pulverizer, and sieving by a 200- mesh sieve, mixing sieved raw material evenly by a mixer according to mass ratios as follows: A calcium carbide slag, silica fume and phosphogypsum at a mass ratio of 54:20:26 or B calcium carbide slag, silica fume and desulfurized gypsum at a mass ratio of 53:28:19, sieving by a 0.08- mm sieve, and putting in a mold for compression molding, to obtain raw meal; calcining the raw meal, wherein when the raw meal is obtained based on mass ratio A, the calcination is performed at 1200 °C, and when the raw meal is obtained based on mass ratio B, the calcination is performed at 1150 °C; and taking out the calcined product obtained, cooling to room temperature within 20 min, and pulverizing to obtain the calcium sulphosilicate-dicalcium silicate-calcium sulphoaluminate where calcium sulphosilicate is the main component.

Description

METHOD FOR PREPARING CALCIUM SULPHOSILICATE-DICALCIUM SILICATE-CALCIUM SULPHOALUMINATE SYSTEM FROM CALCIUM CARBIDE SLAG, AND METHOD FOR IMPROVING LATE-STAGE STRENGTH OF CEMENT
TECHNICAL FIELD
100011 The present disclosure belongs to the technical field of building materials, and in particular to a method for preparing a C5S2 g-C7S-C4A3 S system from a calcium carbide slag, and a method for improving late-stage strength of cement
BACKGROUND ART
[0002] Sulphoaluminate cement is a hydraulicity cementitious material made by grinding clinker with an appropriate amount of gypsum. The clinker is composed of anhydrous calcium sulphoaluminate and dicalcium silicate as main minerals, and is prepared by calcining limestone, bauxite and gypsum in appropriate proportions at low temperature (1300 °C-1350 °C). At present, sulphoaluminate cement has become the largest scale non-silicate special cement in China, with annual production and consumption of nearly 2.2 million tons. Sulphoaluminate cement is widely used in various special projects such as winter construction, rapid construction, repair and renovation, marine and underground due to the performances such as high early strength, fast condensation rate, low alkalinity, micro-expansion, and excellent corrosion resistance and frost resistance. Although having the excellent performances, sulphoaluminate cement still has performance deficiencies such as slow strength growth in the later stage, difficult adjustment of condensation time and unstable expansion. In response to the above problems, most researchers reduce the water-cement ratio while ensuring a certain working performance of the cement by adding water-reducing agents, such as sulfonated melamine resin and naphthalene-based water-reducing agents to the cement. Other scholars have prepared and explored a high belite sulphoaluminate cement by calcining at 1300°C to 1350 °C. This cement delays the phenomenon of excessively rapid condensation to a certain extent, but still has a slow late-stage strength development.
[0003] Silicate-sulphoaluminate cement is a compound of silicate cement and sulphoaluminate cement, integrating the advantages of the two types of cement. Silicate-sulphoaluminate cement not only has the advantages such as quick hardening and early strengthening and desirable impermeability, but also has high late-stage strength, both performances are well complementary. Researches of the silicate-sulphoaluminate cement show that the silicate-sulphoaluminate cement composite system has performances better than those of the single cement, and obviously improves the performance of traditional cement after mixing, thereby better and higher meeting the actual construction needs.
[0004] Yan Shen et al. found a promotion effect of calcium sulphosilicate on the sulphoaluminate cement. The calcium sulphosilicate (4Ca0-2Si02-CaSO4) is a transition mineral during the calcination of the sulphoaluminate cement clinker. The calcium sulphosilicate mineral has an optimum formation temperature of 1050 °C to 1200 °C, and will decompose into C2S and CaSO4 when exceeding 1250 °C. In the past, the calcium sulphosilicate mineral was considered to be an inert mineral, and its formation was avoided in traditional sulphoaluminate cement production; however, later studies found that A1(OH)4-produced by hydration of calcium sulphoaluminate in the sulphoaluminate cement has a significant stimulating effect on the hydration activity of the calcium sulphoaluminate. Moreover, the calcium sulphosilicate releases gypsum during the hydration process, which further promotes the formation and stabilization of ettringite, while the mechanical properties of cement are also significantly improved. This solves the problems of early micro-expansion, and late-stage insufficient strength accumulation and the low growth rate of the sulphoaluminate cement.
[0005] In previous studies, the sulphoaluminate cement clinker containing calcium sulphosilicate prepared by directly reducing the temperature affected the late-stage strength of cement; meanwhile, there was a certain economic cost problem in the preparation of the calcium sulphosilicate using pure drugs. Therefore, the present disclosure proposes to synthesize the calcium sulphosilicate mineral using a calcium carbide slag, to improve the strength of traditional sulphoaluminate cement or silicate-sulphoaluminate cement.
SUMMARY
[0006] In view of the drawbacks in the prior art, in the present disclosure, a C5S2 S-C2S-C4A3 S system is prepared by calcinating waste slags with convenient material access and low cost, such as calcium carbide slag, and added into sulphoaluminate cement or a silicate-sulphoaluminate composite cement according to a certain proportion. Thus, the system improves and maintains the late-stage strength of the cement, and is convenient for large-scale production and use in engineering technology.
[0007] The present disclosure provides the following technical solutions: [0008] Preparation of raw meal: calculating the ratios of the raw materials according to the stoichiometric formula of calcium sulphosilicate (4Ca0.2Sith*CaSO4) and the Bogue formula, and the ratios are as follows: a mass ratio of calcium carbide slag, silica fume and phosphogypsum is 54:20:26, and C) a mass ratio of calcium carbide slag, silica fume and desulfurized gypsum is 53:28:19, mixing the raw materials evenly by a mixer according to one of the mass ratios, sieving by a 0.08-mm square-hole sieve, and putting into a mold for compression molding; [0009] (1) drying three raw materials in an oven at 100 °C for more than 24 h, such that the moisture in the raw materials is fully volatilized, and mixing evenly by the mixer according to the calculated raw material ratios, and taking out to obtain raw meal; [0010] (2) calcination: putting the mixed raw meal into the mold for compression molding, and calcining at three temperatures of 1150 °C, 1175 °C, and 1200°C respectively for 2 h, and hold for 2 h, taking out, and air-cooling to room temperature; [0011] (3) grinding the cooled raw meal by a ball mill until the fineness reaches 200-mesh sieve, and the sieve residue is less than or equal to 10%, to obtain calcium sulphosilicate mineral; and [0012] (4) subjecting the obtained calcium sulphosilicate to X-Ray diffraction (XRD) quantitative and quantitative analysis to obtain a mineral component.
[0013] In the present disclosure, the C5S2 S-C2S-C4A3 S system is a powdered solid product with calcium sulphosilicate as the main component.
[0014] In the present disclosure, the raw materials used are all industrial waste slags such as calcium carbide slag, silica fume and phosphogypsum; given that the waste slag further contains other minerals such as alumina, magnesia and sodium oxide, these impurity phases as a mineralizer are more beneficial to the synthesis of calcium sulphosilicate.
[0015] In the present disclosure, the sintered product contains maximum content of 87.26% of the calcium sulphosilicate, 6% to 25% of dicalcium silicate, and a small amount of anhydrous calcium sulphoaluminate.
[0016] In the present disclosure, the C5S2 S-C2S-C4A3 S system has a formation temperature of 1050°C to 1200°C, and the C5S2 S-C2S-C4A3 S system prepared from the calcium carbide slag raw material has an optimum temperature of 1200°C, and has a holding time of 2 h. This facilitates the production of calcium sulphosilicate with higher purity.
[0017] In some embodiments, the gypsum can also be selected as desulfurized gypsum that has low cost and cheap implementation.
[0018] In some embodiments, the prepared calcium sulphosilicate mineral contains a mass fraction of 40% to 90% of the calcium sulphosilicate, and a mass fraction of 10% to 40% of the dicalcium silicate; the dicalcium silicate and a small amount of a belite component contained in the prepared mineral have a beneficial effect on improving the late-stage strength of sulphoaluminate cement.
[0019] The present disclosure has the following advantages: [0020] (1) In the present disclosure, the C5S2 -C7S-C4A3 S system prepared from the calcium carbide slag and the method for improving the late-stage strength of sulphoaluminate cement is used to improve the strength of traditional sulphoaluminate cement or silicate-sulphoaluminate cement and improve the performance of traditional cement. The methods have a simple synthesis process, low operation difficulty coefficient and abundant and wide range of raw materials. The present disclosure not only solves the problems of environmental pollution and a large number of stockpiles, but also effectively utilizes resources and improves the physical properties of sulphoaluminate cement.
100211 (2) In the present disclosure, the optimal calcination temperature, holding time, and corresponding purity was obtained by preparing the C5S2 S-C9S-C4A3 S mineral system from calcium carbide slag calcareous raw materials contribute to the reference of future research experiments.
100221 (3) The C5S2 S-C2S-C4A3 S mineral system is added into the sulphoaluminate cement as an additive, and reacts with other minerals to form CSH gel and ettringite after hydration and dissolution. The system promotes the increase of the strength of sulphoaluminate cement, solves the problems of the insufficient strength accumulation in the later stage of sulphoaluminate cement, and improves the growth rate of cement strength in the later stage. In addition, the system also reduces the influence of drying shrinkage of sulphoaluminate cement on the volume stability of the cement itself, improves deficiencies in the use of the sulphoaluminate cement, and promotes large-scale production and the use of sulphoaluminate cement.
[0023] (4) The calcined product of this mineral system contains a small amount of the belite component, which has a favorable effect on the late-stage strength of sulphoaluminate cement after the hydration of dicalcium silicate.
DETAILED DESCRIPTION OF THE EMBODIMENTS
[0024] The present disclosure will be further described below with reference to the specific examples.
[0025] Example 1
100261 A method for preparing a C5S2 S-C9S-C4A3 S system from a calcium carbide slag, and a method for improving late-stage strength of cement were performed by the following steps: the amount of calcium carbide slag, silica fume and phosphogypsum in percentages by mass were calculated according to the Bogue formula: 54% of calcium carbide slag, 20% of silica fume, and 26% of phosphogypsum. The raw materials were ground to a fineness of 100 mesh to 200 mesh, mixed evenly, and subjected to compression molding, and calcined at 1150 °C, 1175 °C, and 1200 °C respectively for 2 h, and then held for 2 h, obtaining a calcined product. The calcined product was taken out and air-cooled to room temperature, and then ground by a ball mill to a fineness of 200 mesh and the sieve residue of less than 10%, obtaining a powdery mineral component with calcium sulphosilicate as the main component [0027] An X-ray diffraction measurement experiment was carried out on the mineral with calcium sulphosilicate as the main component synthesized in the above-mentioned Example 1, and the content of each component was quantitatively measured by TOPAS. It was determined that at a temperature of 1200 °C, the mineral had maximum content of calcium sulphosilicate, in which the content of calcium sulphosilicate was 87.26% by mass, the content of dicalcium silicate was 9.88% by mass, and the content of anhydrous calcium sulphoaluminate was 0.62% by mass.
[0028] Example 2
[0029] A method for preparing a C5S2 S-C2S-C4A3 S system from a calcium carbide slag, and a method for improving late-stage strength of cement were performed by the following steps: the amount of calcium carbide slag, silica fume and desulfurized gypsum in percentages by mass were calculated according to the Bogue formula:53% of calcium carbide slag, 28% of silica fume, and 19% of desulfurized gypsum, in which the desulfurized gypsum was the optimal choice of cost economy of gypsum. The raw materials were ground to a fineness of 100 mesh to 200 mesh, mixed evenly, and subjected to compression molding, and calcined at 1150 °C, 1175 °C, and 1200 °C respectively for 2 h, and then held for 2 h, obtaining a calcined product. The calcined product was taken out and air-cooled to room temperature, and then ground by a ball mill to a fineness of 200 mesh and the sieve residue of less than 10%, obtaining a powdery mineral component with calcium sulphosilicate as the main component.
[0030] An X-ray diffraction measurement experiment was carried out on the mineral with calcium sulphosilicate as the main component synthesized in the above-mentioned Example 2, and the content of each component was quantitatively measured by TOPAS. It was determined that at a temperature of 1150 °C, the mineral had maximum content of the calcium sulphosilicate, in which the content of calcium sulphosilicate was 67.34% by mass, the content of dicalcium silicate was 22.72% by mass, and the content of anhydrous calcium sulphoaluminate was 3.60% by mass.
[0031] In order to further verify the improvement effect of the mineral system prepared from calcium carbide slag calcareous raw material according to the present disclosure on the late-stage strength of sulphoaluminate cement during use, the performance of the cement additive products prepared in Examples 1 and 2 were verified.
[0032] During the experiment, the sulphoaluminate cement was taken as a cementitious material, and the calcium sulphosilicate mineral prepared in the example was added according to a mass ratio of 12%, and the resulting mixture was prepared into cement specimen according to a standard. Meanwhile, a group of cement without calcium sulphosilicate was set as a comparison reference The strength measured according to the national standard GB/T 17671-1999 "Method of Testing Cements, Determination of Strength" was shown in the following table.
[0033] Table 1 Compressive strength [0034] Compressive strength / MPa Id 3d 7d 28d 56d Control 52.62 60.88 59.97 64.62 54.51 Example 1 35.33 45.91 47.09 57.40 58.01 Example 2 39.67 41.67 50.01 62.54 65.19

Claims (2)

  1. WHAT IS CLAIMED IS: 1. A method for preparing a calcium sulphosilicate-d calc um silicate-calcium sulphoaluminate system from a calcium carbide slag, comprising: (1) preparation of raw meal: grinding calcium carbide slag, silica fume, and one of phosphogypsum and desulfurized gypsum by a pulverizer, and sieving by a 200-mesh sieve, mixing sieved raw material evenly by a mixer according to mass ratios as follows: calcium carbide slag, silica fume and phosphogypsum at a mass ratio of 54:20:26 or (?), calcium carbide slag, silica fume and desulfurized gypsum at a mass ratio of 53:28:19, sieving by a 0.08-mm square-hole sieve, and putting in a mold for compression molding, to obtain raw meal; (2) calcination: calcining the raw meal obtained in (1), and holding, wherein when the raw meal is obtained based on mass ratio OD, the calcination is performed at 1200 °C, and when the raw meal is obtained based on mass ratio ©, the calcination is performed at 1150 °C; and (3) cooling: taking out the calcined product obtained in (2), cooling to room temperature within 20 min, and pulverizing to obtain the mineral with calcium sulphosilicate as the main component.
  2. 2. A method for improving late-stage strength of cement by using the system according to claim 1, comprising: using the calcium sulphosilicate prepared in claim 1 as an additive, and using sulphoaluminate cement as a base material, and the amount of raw materials added in percentages by mass: 80% of sulphoaluminate cement, 5% to 15% of calcium sulfosilicate, and 5% to 15% of anhydrite, and the raw materials have a total mass percentage of 100%.
GB2203020.9A 2021-03-05 2022-03-04 Method for preparing calcium sulphosilicate-dicalcium silicate-calcium sulphoaluminate system from calcium carbide slag and method for improving late-stage Pending GB2607658A (en)

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CN112960929A (en) * 2021-03-05 2021-06-15 北京工业大学 Method for preparing calcium sulfosilicate-dicalcium silicate-calcium sulfoaluminate system from calcium carbide slag raw material and improving later strength of cement
CN115849740B (en) * 2022-12-07 2024-03-29 中国建筑材料科学研究总院有限公司 Dicalcium silicate-calcium sulfoaluminate-calcium sulfosilicate cement clinker and preparation process thereof
CN116354744B (en) * 2023-04-28 2024-03-01 湖北工业大学 Titanium dioxide antibacterial self-cleaning baking-free glaze and application method thereof
CN118125735B (en) * 2024-05-08 2024-06-28 常熟理工学院 Method for preparing thallium-rich powder and cement gel powder by cooperatively utilizing lithium slag and oil sludge

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CN104609750A (en) * 2015-02-09 2015-05-13 重庆大学 Sulphoaluminate cement and preparation method thereof
CN110498631A (en) * 2019-08-30 2019-11-26 北京工业大学 A method of improving sulphate aluminium cement stable long-term strength
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