CN107117838B - Sulphate aluminium cement clinker containing tricalcium silicate and preparation method thereof - Google Patents

Sulphate aluminium cement clinker containing tricalcium silicate and preparation method thereof Download PDF

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CN107117838B
CN107117838B CN201710390145.0A CN201710390145A CN107117838B CN 107117838 B CN107117838 B CN 107117838B CN 201710390145 A CN201710390145 A CN 201710390145A CN 107117838 B CN107117838 B CN 107117838B
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cement clinker
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sulphoaluminate
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CN107117838A (en
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程新
叶正茂
卢晓磊
李传海
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University of Jinan
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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
    • 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
    • C04B7/36—Manufacture of hydraulic cements in general
    • C04B7/38—Preparing or treating the raw materials individually or as batches, e.g. mixing with fuel
    • C04B7/42—Active ingredients added before, or during, the burning process
    • C04B7/421—Inorganic materials
    • C04B7/424—Oxides, Hydroxides
    • 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
    • C04B7/36—Manufacture of hydraulic cements in general
    • C04B7/43—Heat treatment, e.g. precalcining, burning, melting; Cooling
    • C04B7/44—Burning; Melting
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    • 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
    • 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
    • Y02P40/121—Energy efficiency measures, e.g. improving or optimising the production methods

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  • Ceramic Engineering (AREA)
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  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

The invention relates to a sulphoaluminate cement clinker containing tricalcium silicate and a preparation method thereof, wherein in the mineral composition, the iron phase is 2 CaO. Fe2O3(C2F) (ii) a The sulphoaluminate mineral is 3 CaO.3Al2O3·BaSO4(C3BA3$ h); the mineral composition in percentage by weight is as follows: c3S 5～30％，C3BA3$ 20～65％，C2S 30～60％，C2F3-25%; wherein, the oxides are abbreviated as C = CaO, S = SiO2、A=Al2O3、F=Fe2O3、$=SO3B = BaO. By adjusting the composition of iron phase and adopting the ion doping technology, the introduction of C into the sulphoaluminate cement clinker is successfully realized3S mineral, preparing C-containing3S, sulphoaluminate cement clinker. The invention has low limestone consumption and low requirement on limestone grade; avoids the traditional mineralizer CaF2The environment is polluted and the cement kiln system is corroded; at the same time due to the introduction of C3S improves the alkalinity of the system, increases the mixing amount of the mixed material and has important significance in the field of green manufacture and application of cement.

Description

Sulphate aluminium cement clinker containing tricalcium silicate and preparation method thereof
Technical Field
The invention relates to the technical field of cement material preparation, in particular to a cement material containing C3S sulphoaluminate cement clinker and a preparation method thereof.
Background
The sulphoaluminate cement is a cementing material with the properties of early strength, high impermeability and micro-expansion, and the main mineral thereof is calcium sulphoaluminate (C)4A3C) in the clinker system, the temperature at which the clinker is formed in large quantities is about 1200 ℃ and at higher temperatures4A3And decomposes, and is generally considered to exist stably at an upper temperature of 1350 ℃. Portland cement clinker main mineral phase tricalcium silicate (C)3S) is in the presence of a liquid phaseFormed at a temperature of at least 1250 ℃ C3The bulk formation temperature of S is generally above 1350 ℃. And high SO is present in the clinker system3At a content of C, C is inhibited3S mineral formation, and therefore, in general, C3S cannot be present in the sulphoaluminate cement clinker. The oxides are abbreviated as: c = CaO, S = SiO2、A=Al2O3、F=Fe2O3、$=SO3、B=BaO。
Prior art introduction of C into sulphoaluminate cement clinker3S mineral, essentially by adding mineralizer CaF to clinker system2Decrease C3S firing temperature, thereby realizing C3S is introduced into the sulphoaluminate cement clinker system. Patent calcium sulphoaluminate-alite composite mineral phase cement clinker and preparation method thereof (publication No. CN 1951853A) and patent C3The S-type sulphoaluminate cement clinker and the preparation method (CN 104326687A) both use a mineralizer CaF2Implementation C3S and C4A3And $ coexist. But mineralizer CaF2Can cause environmental pollution, is corrosive to a cement kiln system and simultaneously has the following performance of CaF2The increase of the mixing amount can have adverse effects on the performance of the cement, and the application of the cement in the preparation of cement clinker is limited.
Thus, a novel C-containing compound was developed3The research of the sulphoaluminate cement clinker of S and the preparation method thereof has important significance for the industrial development of the clinker.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provide a sulphoaluminate cement clinker containing tricalcium silicate, which adopts CaCO3、BaCO3、SiO2、Al(OH)3、Fe2O3And CaSO4·2H2O is taken as a raw material, and the problem of introducing C into the sulphoaluminate cement clinker is solved3S mineral problem.
The invention also provides a preparation method of the tricalcium silicate-containing sulphoaluminate cement clinker, which is used for preparing the cement clinker by adjusting the composition and the content of an iron phase of a clinker system and adopting an ion doping technologyContaining tricalcium silicate (C)3S) sulphoaluminate cement clinker.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a sulphoaluminate cement clinker containing tricalcium silicate is composed of minerals containing iron phase C2F; the sulphoaluminate mineral is C3BA3$；
Said C is2F, dicalcium ferrite, of the stoichiometric formula 2 CaO. Fe2O3(ii) a Said C is3BA3Barium calcium sulphoaluminate with the stoichiometric proportion of 3 CaO.3 Al2O3·BaSO4。
The tricalcium silicate-containing sulphoaluminate cement clinker comprises the following mineral components in percentage by weight:
C3S 5～30％，
C3BA3$ 20～65％，
C2S 30～60％，
C2F 3～25％；
wherein, the oxides are abbreviated as C = CaO, S = SiO2、A=Al2O3、F=Fe2O3、$=SO3、B=BaO。
The sulphoaluminate cement clinker containing tricalcium silicate comprises the following chemical components in percentage by weight:
CaO 47～60%，
SiO211～29%，
Al2O38～28%，
Fe2O31～15%，
BaO 5～17%，
SO32～8%。
the preparation method of the sulphoaluminate cement clinker containing tricalcium silicate comprises the following steps:
1) preparing materials: weighing the raw material CaCO according to the following weight parts383 to 107 parts of BaCO36.4 to 21.8 parts of SiO211 to 29 parts of Al (OH)312.2 to 43.8 parts of Fe2O31-15 parts of and CaSO4·2H24.3-17.2 parts of O, and then mixing the prepared raw materials by a wet method, drying and tabletting for later use;
2) and (3) calcining: heating the raw materials treated in the step 1) from room temperature to 900 ℃ at a speed of 5 ℃/min, then carrying out heat preservation and calcination for 1h, heating to 1300-1410 ℃ at a speed of 3 ℃/min, and carrying out heat preservation and calcination for 0.5-1.5 h;
3) and (3) cooling: after calcining and sintering, air quenching is carried out to obtain the sulphoaluminate cement clinker containing tricalcium silicate.
Preferably, in step 1), the particle size of the raw material is below 80 μm.
Preferably, in step 1), the drying temperature is 105 ℃.
Preferably, in step 1), the tabletting method comprises the following steps: adding 7% water into the dried raw materials, uniformly mixing, pressing in a steel die under 16 MPa to obtain raw material slices with phi 35 mm multiplied by 5 mm, and then drying at 105 ℃ for 4 h.
Preferably, in the step 2), the temperature is increased to 1320 ℃ at 3 ℃/min, and the calcination is carried out for 1h under the condition of heat preservation.
The liquid phase of the sulphate aluminium cement clinker containing tricalcium silicate of the invention is mainly composed of CaO and Al in the calcining process2O3And Fe2O3Isocomposition, clinker sintering to form C3S process, temperature of formation of liquid phase, amount of liquid phase, nature of liquid phase, CaO and C2The dissolution rate of S in the liquid phase, the ion diffusion rate, and the like. Therefore, by adjusting the composition and content of the iron phase and adopting the ion doping technology, the problem of generating a certain amount of C in the sulphoaluminate cement clinker is solved3And (5) S mineral. Thereby avoiding the introduction of CaF2Impact on cement properties and equipment. C-containing cement with continuously increased middle and later strength is prepared by regulating and controlling the liquid phase property of a clinker system3S, and overcomes the problem that the use of the admixture is limited due to low alkalinity of the sulphoaluminate cement.
The raw material minerals of the sulphate aluminium cement clinker containing tricalcium silicate of the invention all adopt CaCO3、BaCO3、SiO2、Al(OH)3、Fe2O3And CaSO4·2H2O proportioning and sintering clinker to form C3The process of S requires a liquid phase environment, and the invention designs the iron phase composition into C2F, the iron phase amount is between 3 and 25 percent, and C can be effectively promoted2More S is dissolved in liquid phase and absorbs CaO to be converted into C3S, BaO is introduced to raise the decomposition temperature of sulphoaluminate mineral by 30 deg.C and enlarge C3The temperature coexistence interval of the S and the sulphoaluminate mineral.
The technical scheme of the invention has the beneficial effects and characteristics that:
1) by adjusting the composition of iron phase, C can be obviously reduced3The formation temperature of S minerals is favorable for energy conservation and consumption reduction.
2) The sulphoaluminate mineral in the sulphoaluminate cement clinker containing tricalcium silicate is barium calcium sulphoaluminate (3 CaO.3Al)2O3·BaSO4) Its decomposition temperature is lower than C4A3The height is 30 ℃, enlarge C3The coexisting interval of S and sulphoaluminate minerals.
3) The sulphoaluminate cement clinker containing the tricalcium silicate can increase the mixing amount of the mixed materials in the sulphoaluminate cement.
Drawings
FIG. 1 is an XRD pattern of the mineral composition of a tricalcium silicate-containing sulphoaluminate cement clinker prepared in example 1;
FIG. 2 is an XRD pattern of the mineral composition of a tricalcium silicate-containing sulphoaluminate cement clinker prepared in example 2;
FIG. 3 is an XRD pattern of the mineral composition of a tricalcium silicate-containing sulphoaluminate cement clinker prepared in example 3;
FIG. 4 is a mineral composition XRD pattern of the cement clinker prepared in comparative example 1;
FIG. 5 is a mineral composition XRD pattern of the cement clinker prepared in comparative example 2;
FIG. 6 is a mineral composition XRD pattern of the cement clinker prepared in comparative example 3.
Detailed Description
The invention will be further illustrated by the following examples for a better understanding of the invention, but the present disclosure is not to be considered as limiting the scope of the invention.
Example 1
A preparation method of sulphate aluminium cement clinker containing tricalcium silicate comprises the following steps:
1) preparing materials: weighing the raw material CaCO according to the following weight parts389.8 parts of BaCO36.4 parts of SiO218.6 parts, Al (OH)315.2 parts of Fe2O311.7 parts of and CaSO4·2H25.6 portions of O, the granularity of each raw material is below 80 mu m, then the prepared raw materials are dried at 105 ℃ after being mixed by a wet method, water with the mass fraction of 7 percent is added, after being mixed evenly, raw material slices with the diameter of 35 mm multiplied by 5 mm are pressed in a steel die under the pressure of 16 MPa, and then the raw material slices are dried for 4 hours at 105 ℃ for standby;
2) and (3) calcining: heating the raw materials treated in the step 1) from room temperature to 900 ℃ at the speed of 5 ℃/min, then carrying out heat preservation calcination for 1h, heating to 1320 ℃ at the speed of 3 ℃/min, and carrying out heat preservation calcination for 1 h;
3) and (3) cooling: after calcining and sintering, air quenching is carried out to obtain the sulphoaluminate cement clinker containing tricalcium silicate.
Example 1 a sulphoaluminate cement clinker containing tricalcium silicate, the mineral content percentage composition of which is: c3S 15%，C2S42%，C2F 20%，C3BA3$ 23%. Wherein, the oxides are abbreviated as C = CaO, S = SiO2、A=Al2O3、F=Fe2O3、$=SO3B = BaO. The mineral composition of the obtained clinker sample is shown in XRD spectrum of figure 1, and it can be seen that iron phase is C in the mineral composition2F; the sulphoaluminate mineral is C3BA3$；
The chemical composition and percentage content are as follows: CaO 52.1%, SiO218.6%，Al2O39.9%，Fe2O311.8%，BaO5.0%，SO32.6%。
Example 2
A preparation method of sulphate aluminium cement clinker containing tricalcium silicate comprises the following steps:
1) preparing materials: weighing the raw material CaCO according to the following weight parts391.9 parts of BaCO36.4 parts of SiO220.4 parts of Al (OH)315.2 parts of Fe2O38.8 parts of and CaSO4·2H25.6 portions of O, the granularity of each raw material is below 80 mu m, then the prepared raw materials are dried at 105 ℃ after being mixed by a wet method, water with the mass fraction of 7 percent is added, after being mixed evenly, raw material slices with the diameter of 35 mm multiplied by 5 mm are pressed in a steel die under the pressure of 16 MPa, and then the raw material slices are dried for 4 hours at 105 ℃ for standby;
2) and (3) calcining: heating the raw materials treated in the step 1) from room temperature to 900 ℃ at the speed of 5 ℃/min, then carrying out heat preservation calcination for 1h, heating to 1350 ℃ at the speed of 3 ℃/min, and carrying out heat preservation calcination for 1 h;
3) and (3) cooling: after calcining and sintering, air quenching is carried out to obtain the sulphoaluminate cement clinker containing tricalcium silicate.
Example 2 a sulphoaluminate cement clinker containing tricalcium silicate, the mineral content of which is: c3S 15%，C2S47%，C2F 15%，C3BA3$ 23%. Wherein, the oxides are abbreviated as C = CaO, S = SiO2、A=Al2O3、F=Fe2O3、$=SO3B = BaO. The mineral composition of the obtained clinker sample is shown in XRD spectrum of figure 2, and it can be seen that iron phase is C in the mineral composition2F; the sulphoaluminate mineral is C3BA3$；
The chemical composition and percentage content are as follows: CaO 53.3%, SiO220.4%，Al2O39.9%，Fe2O38.8%，BaO5.0%，SO32.6%。
Example 3
A preparation method of sulphate aluminium cement clinker containing tricalcium silicate comprises the following steps:
1) preparing materials: weighing the raw material CaCO according to the following weight parts386.3 parts of BaCO37.5 parts of SiO217.2 parts, Al (OH)317.9 parts of Fe2O311.7 parts of and CaSO4·2H2O6.6 portions, the granularity of each raw material is below 80 mu m, then the prepared raw materials are mixed by a wet method, dried at 105 ℃, added with water with the mass fraction of 7 percent, mixed evenly and pressed into phi 35 mm multiplied by 5 under the pressure of 16 MPa in a steel dieBaking the mm raw material slices at 105 ℃ for 4h for later use;
2) and (3) calcining: heating the raw materials treated in the step 1) from room temperature to 900 ℃ at a speed of 5 ℃/min, then carrying out heat preservation calcination for 1h, heating to 1380 ℃ at a speed of 3 ℃/min, and carrying out heat preservation calcination for 1 h;
3) and (3) cooling: after calcining and sintering, air quenching is carried out to obtain the sulphoaluminate cement clinker containing tricalcium silicate.
Example 3a sulphoaluminate cement clinker containing tricalcium silicate, the mineral content of which is: c3S 15%，C2S38%，C2F 20%，C3BA3$ 27%. Wherein, the oxides are abbreviated as C = CaO, S = SiO2、A=Al2O3、F=Fe2O3、$=SO3B = BaO. The mineral composition of the obtained clinker sample is shown in XRD spectrum of figure 3, wherein C is clearly shown3Diffraction peak of S (d ═ 1.76) and C3BA3$ ( d＝3.77 )。
The chemical composition and percentage content are as follows: CaO 50.5%, SiO217.2%，Al2O311.7%，Fe2O311.7%，BaO 5.8%，SO33.1%。
Comparative example 1
The preparation method is the same as the example 1, except that the ingredients in the step 1) comprise: weighing the raw material CaCO according to the following weight parts394.6 parts of SiO218.6 parts, Al (OH)317.6 parts of Fe2O311.7 parts of and CaSO4·2H2And 6.5 parts of O.
The cement clinker obtained in the comparative example 1 comprises the following minerals in percentage by weight: is mainly C2S，C2F，C4A3And free calcium, no C is found3S characteristic diffraction peak (d ═ 1.76); the mineral composition of the obtained clinker sample is shown in XRD spectrum of figure 4, and it can be seen that iron phase is C in the mineral composition2F; the sulphoaluminate mineral is C4A3$。
Comparative example 2
The preparation method is the same as the example 2, except that the ingredients in the step 1 comprise: CaCO398.0 parts of SiO220.3 parts of Al (OH)322.5 parts of Fe2O34.9 parts of and CaSO4·2H2And 6.5 parts of O.
The cement clinker obtained in the comparative example 2 comprises the following minerals in percentage by weight: is mainly C2S，C4AF， C4A3And free calcium, no C is found3S characteristic diffraction peak (d ═ 1.76);
the mineral composition is shown in XRD spectrum of figure 5, and the iron phase is C4AF; the sulphoaluminate mineral is C4A3$。
Comparative example 3
The preparation method is the same as example 1, except that the step 1): weighing the raw material CaCO according to the following weight parts394.6 parts of SiO218.6 parts, Al (OH)317.6 parts of Fe2O311.7 parts of and CaSO4·2H2O6.5, mixing the prepared raw materials by a wet method, drying and tabletting for later use;
heating the raw materials treated in the step 1) from room temperature to 900 ℃ at the speed of 5 ℃/min, then carrying out heat preservation calcination for 1h, heating to 1380 ℃ at the speed of 3 ℃/min, and carrying out heat preservation calcination for 1 h.
The cement clinker obtained in the comparative example 3 comprises the following minerals in percentage by weight: is mainly C2S，C2F，C4A3And free calcium, no C found3S characteristic diffraction peak; the mineral composition of the obtained clinker sample is shown in XRD spectrum of figure 6, and it can be seen that iron phase is C in the mineral composition2F; the sulphoaluminate mineral is C4A3$。

Claims (4)

1. A sulphoaluminate cement clinker containing tricalcium silicate is characterized in that: in the mineral composition, the iron phase is C2F; the sulphoaluminate mineral is C3BA3$ 3; said C is2F, dicalcium ferrite, of the stoichiometric formula 2 CaO. Fe2O3(ii) a Said C is3BA3Barium calcium sulphoaluminate, with the stoichiometric formula 3 CaO.3 Al2O3·BaSO4；
The sulphoaluminate cement clinker comprises the following minerals in percentage by weight:
C3S 5～15％，
C3BA3$ 20～27％，
C2S 30～47％，
C215-20% of F, wherein the sum of the percentage contents of the mineral compositions is 100%;
wherein, the oxides are abbreviated as C = CaO, S = SiO2、A=Al2O3、F=Fe2O3、$=SO3、B=BaO；
The preparation method of the sulphoaluminate cement clinker comprises the following steps:
1) preparing materials: weighing the raw material CaCO according to the following weight parts383 to 107 parts of BaCO36.4 to 21.8 parts of SiO211 to 29 parts of Al (OH)312.2 to 43.8 parts of Fe2O31-15 parts of and CaSO4·2H24.3-17.2 parts of O, and then mixing the prepared raw materials by a wet method, drying and tabletting for later use;
2) and (3) calcining: heating the raw materials treated in the step 1) from room temperature to 900 ℃ at a speed of 5 ℃/min, then carrying out heat preservation and calcination for 1h, heating to 1300-1410 ℃ at a speed of 3 ℃/min, and carrying out heat preservation and calcination for 0.5-1.5 h;
3) and (3) cooling: after calcining and sintering, air quenching is carried out to obtain the sulphoaluminate cement clinker containing tricalcium silicate.
2. The sulfoaluminate cement clinker of claim 1, wherein: the chemical composition and percentage content are as follows:
CaO 47～53.3%，
SiO211～20.4%，
Al2O38～11.7%，
Fe2O31～11.8%，
BaO 5～5.8%，
SO32～3.1%;
the sum of the percentage contents of the chemical compositions is 100 percent.
3. The sulfoaluminate cement clinker of claim 1, wherein: in step 1), the particle size of the raw material is below 80 μm.
4. The sulfoaluminate cement clinker of claim 1, wherein: in the step 2), the temperature is increased to 1320 ℃ at 3 ℃/min, and the heat preservation and calcination are carried out for 1 h.
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《微量元素对阿利特-硫铝酸钡钙水泥制备工艺及性能的影响》;于丽波;《万方学位论文》;20051116;第5页倒数第1段-第6页第1段、第8页第4段、第12页第1-4段及第33页第3段-第34页表5-1 *

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