CN115710095A - Boron-phosphorus composite modified high belite sulphoaluminate cement clinker and preparation method thereof - Google Patents
Boron-phosphorus composite modified high belite sulphoaluminate cement clinker and preparation method thereof Download PDFInfo
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- CN115710095A CN115710095A CN202211593943.0A CN202211593943A CN115710095A CN 115710095 A CN115710095 A CN 115710095A CN 202211593943 A CN202211593943 A CN 202211593943A CN 115710095 A CN115710095 A CN 115710095A
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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
- 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
Abstract
A boron-phosphorus composite modified high belite sulphoaluminate cement clinker and a preparation method thereof. Relates to the field of building materials. The technical scheme of the invention is as follows: the cement clinker comprises the following raw materials in percentage by mass: 55 to 70 percent of limestone, 12 to 20 percent of sandstone, 0 to 5 percent of Bayer process red mud, 5 to 15 percent of desulfurized gypsum, 5 to 15 percent of bauxite, 0.01 to 1 percent of borax and 0.01 to 2 percent of calcium phosphate. The minerals in the cement clinker comprise the following components in percentage by mass: c 4 A 3 $:15%～30%,C 2 $:55%～75%,C 4 5 to 10 percent of AF, 5 to 20 percent of C and the balance of mixed mineralsAnd (3) preparing. The invention has the advantages that: borax and calcium phosphate are added into the raw material of the high belite sulphoaluminate cement, so that dicalcium silicate in the clinker minerals is formed by beta-C 2 Conversion of S crystal form to more active alpha-C 2 S and alpha' -C 2 The crystal form S enables the hydration process of dicalcium silicate to be advanced, and the later strength is effectively improved.
Description
Technical Field
The invention relates to the field of building materials, in particular to a boron-phosphorus composite modified high belite sulphoaluminate cement clinker and a preparation method thereof.
Background
The sulphoaluminate cement is a new type of low carbon cement, the firing temperature is 100-150 deg.C lower than that of silicate cement, and its carbon emission is far lower than that of silicate cement. However, the main reason for the problems of difficult construction due to too short setting time and difficult increase and even collapse of later-stage strength of the sulphoaluminate cement is that calcium sulphoaluminate, the main mineral of the sulphoaluminate cement, reacts quickly in the early-stage hydration process to generate high-sulfur hydrated calcium sulphoaluminate (ettringite), and the mineral is gradually converted into monosulfur hydrated calcium sulphoaluminate (AFm) along with the time, so that the later-stage strength is increased and weakened, even the strength collapses, and the requirement of later-stage hydration strength increase cannot be met. Therefore, how to ensure the stable development of the middle and later strength of the sulphoaluminate cement becomes a problem to be solved urgently.
The high belite sulphoaluminate cement is a novel cement which can effectively solve the problems and is mainly different from the traditional sulphoaluminate cement in lower C 4 A 3 C and higher 2 The S mineral accounts for and the clinker has low aluminum content, so that bauxite with lower grade can be used as the aluminum raw material, and the utilization rate of the raw material is improvedAnd the production cost is reduced. Compared with silicate cement clinker, CO in the production process of the cement clinker 2 The emission amount is lower. In addition, the high belite sulphoaluminate cement ensures stable later strength increase of clinker while maintaining high early strength of common sulphoaluminate cement.
However, most high belite sulphoaluminate cements at present do not meet the requirements for strength increase in the middle and later stages, mainly due to the post-hydrated mineral dicalcium silicate (C) 2 S) is mostly beta-C in clinker 2 The S form exists, and the time for starting hydration is generally after the 28d age, during which the strength hardly increases, so that a method is needed to solve the problem of insufficient development of the strength of the high belite calcium sulfoaluminate cement.
Disclosure of Invention
Aiming at the problems, the invention provides a boron-phosphorus composite modified high belite calcium sulfoaluminate cement clinker and a preparation method thereof.
The technical scheme of the invention is as follows: the cement clinker comprises the following raw materials in percentage by mass: 55 to 70 percent of limestone, 12 to 20 percent of sandstone, 0 to 5 percent of Bayer process red mud, 5 to 15 percent of desulfurized gypsum, 5 to 15 percent of bauxite, 0.01 to 1 percent of borax and 0.01 to 2 percent of calcium phosphate.
The minerals in the cement clinker comprise the following components in percentage by mass: c 4 A 3 $:15%～30%,C 2 $:55%～75%,C 4 5 to 10 percent of AF, 5 to 20 percent of C and the balance of mixed mineral components.
A preparation method of boron-phosphorus composite modified high belite sulphoaluminate cement clinker comprises the following steps:
(1) Pretreatment of raw materials:
drying the raw materials at 105 deg.C for 24 hr, respectively crushing with a crusher, and grinding to 0.08mm sieve residue less than 8%;
(2) Premixing raw materials:
mixing 55-70% of limestone, 12-20% of sandstone, 0-5% of Bayer process red mud, 5-15% of desulfurized gypsum, 5-15% of bauxite, 0.01-1% of borax and 0.01-2% of calcium phosphate in a mixing tank, and then mixing in a mixer for 9 hours to obtain raw materials;
(3) Tabletting:
adding ultrapure water with the mass fraction of 8% into the premixed raw material, tabletting and placing in a 105 ℃ environment for drying for 12 hours to obtain a dried raw material test block;
(4) Calcining clinker:
placing the raw material block prepared in the step (3) into a muffle furnace for calcining, raising the temperature to 900 ℃ at the heating rate of 5-10 ℃/min, and preserving the temperature for 0.5-1 h; then quickly transferring the test block to an environment with the temperature of 1250-1350 ℃ and preserving the heat for 1h; and removing clinker after the calcination and quenching to obtain the high belite sulphoaluminate cement clinker.
The invention has the advantages that: borax and calcium phosphate are added into the raw material of the high belite sulphoaluminate cement, so that dicalcium silicate in the clinker minerals is formed by beta-C 2 Conversion of S crystal form to more active alpha-C 2 S and alpha' -C 2 The S crystal form advances the hydration process of dicalcium silicate, and effectively improves the later strength.
Detailed Description
The present invention will be described in further detail with reference to the following examples:
the cement clinker comprises the following raw materials in percentage by mass: 55 to 70 percent of limestone, 12 to 20 percent of sandstone, 0 to 5 percent of Bayer process red mud, 5 to 15 percent of desulfurized gypsum, 5 to 15 percent of bauxite, 0.01 to 1 percent of borax and 0.01 to 2 percent of calcium phosphate.
The main system of the cement clinker provided by the invention is CaO-SiO 2 -Al 2 O 3 -SO 3 -Fe 2 O 3 The quinary system contains phosphorus, boron and other elements contained in the mineral.
The addition of borax and calcium phosphate can ensure that a large amount of beta-C exists in clinker 2 More S is converted into highly active alpha' -C 2 S, the improvement of later-stage strength is effectively guaranteed, the lower shrinkage expansion rate is kept, and the stability of cement can be guaranteed.
The minerals in the cement clinker comprise the following components in percentage by mass: c 4 A 3 $:15%～30%,C 2 $:55%～75%,C 4 5 to 10 percent of AF, 5 to 20 percent of C and the balance of mixed mineral components.
A preparation method of boron-phosphorus composite modified high belite sulphoaluminate cement clinker comprises the following steps:
(1) Pretreatment of raw materials:
drying the raw materials at 105 ℃ for 24 hours respectively, and crushing and grinding the raw materials by using a crusher until the 0.08mm screen residue is less than 8%;
(2) Premixing raw materials:
mixing 55-70% of limestone, 12-20% of sandstone, 0-5% of Bayer process red mud, 5-15% of desulfurized gypsum, 5-15% of bauxite, 0.01-1% of borax and 0.01-2% of calcium phosphate in a mixing tank, and then mixing in a mixer for 9 hours to obtain raw materials;
(3) Tabletting:
adding ultrapure water with the mass fraction of 8% into the premixed raw material, tabletting, and drying at 105 ℃ for 12 hours to obtain a dried raw material test block;
(4) Calcining clinker:
placing the raw material block prepared in the step (3) in a muffle furnace for calcining, raising the temperature to 900 ℃ at the heating rate of 5-10 ℃/min, and preserving the temperature for 0.5-1 h; then quickly transferring the test block to an environment of 1250-1350 ℃ and preserving the heat for 1h; and removing clinker after the calcination and quenching to obtain the high belite sulphoaluminate cement clinker.
When in application, the high belite sulphoaluminate cement clinker in the step (4) is ground to reach the Brinell specific surface area of 390-410 m 2 The gypsum is doped with anhydrite with the same specific surface area to promote hydration reaction and is used as a coagulation regulator, and the specific proportion is as follows: the clinker of the high belite sulphoaluminate cement accounts for 95 to 97 percent by mass, and anhydrite accounts for 3 to 5 percent by mass; grinding the mixture to 380-420m of Boehringer's specific surface area 2 And/kg, namely preparing the belite sulphoaluminate cement.
In the concrete application of the method, the material is selected,
the raw materials and their chemical compositions used in examples 1 to 3 are shown in table 1:
TABLE 1 chemical composition of the raw materials
Example 1:
drying the five raw materials at 105 ℃ for 12h, and then preparing the following components in percentage by weight: preparing raw materials of 65.20% of limestone, 8.93% of bauxite, 13.92% of sandstone, 7.65% of desulfurized gypsum and 3.00% of red mud, then adding 0.3% of borax and 1% of calcium phosphate into the mixed raw materials, weighing 1kg of uniformly mixed raw materials after fully mixing uniformly, and grinding the raw materials in a vibration mill until 5% of residue is sieved in a square hole of 0.075mm to obtain the powdery cement raw material. Adding 8% of water by mass into the powdery cement raw materials, uniformly stirring, putting into a tablet press, pressing into a wafer with the diameter of 235mm, and drying at 105 ℃ for 12h. And taking out the materials, putting the materials into a muffle furnace preheated to 900 ℃ for calcining for 30 minutes, then transferring the materials into an electric furnace at 1290 ℃ for heat preservation for 1 hour, taking out the materials, and rapidly cooling the materials to room temperature by using a fan.
Crushing the cooled cement clinker, and grinding the crushed cement clinker to a specific surface area of 400 +/-20 m by using a ball mill 2 Fineness of/kg. The chemical composition of the cement clinker and the mineral composition of the clinker determined by the XRD diffraction quantitative analysis method are shown in Table 2.
TABLE 2 mineral composition of cement clinker
The results of measuring the physical properties such as strength, thickness and water consumption of the cement clinker mortar and setting time according to the national standard are shown in Table 3.
TABLE 3 physical Properties of Cement Clinker and mortar Strength
Example 2:
drying the five raw materials at 105 ℃ for 12 hours, and then mixing the following components in percentage by weight: 66.67 percent of limestone, 8.54 percent of bauxite, 15.52 percent of sandstone, 6.60 percent of desulfurized gypsum and 0.37 percent of red mud, weighing 5kg of raw materials, uniformly mixing, adding 0.3 percent of borax and 2 percent of calcium phosphate which account for the total weight percent of the mixed materials, and grinding the mixture in a vibration mill until the residue of a square hole with the size of 0.075mm is 5 percent, thus obtaining the powdery cement raw material. Adding 8% of water by mass into the powdery cement raw materials, uniformly stirring, putting into a tabletting machine, pressing into round pieces with the diameter of 235mm, and drying at 105 ℃ for 12h. The materials are taken out and put into a muffle furnace which is preheated to 900 ℃ for calcining for 30 minutes, then the muffle furnace is transferred to an electric furnace of 1290 ℃ for heat preservation for 1 hour, and the materials are taken out and rapidly cooled to the room temperature by a fan.
Crushing the cooled cement clinker, and grinding the crushed cement clinker to 400 +/-20 m of specific surface area by using a ball mill 2 Fineness of/kg. The chemical composition of the cement clinker and the mineral composition of the clinker determined by the XRD diffraction quantitative analysis method are shown in Table 4.
TABLE 4 actual mineral composition of cement clinker
The results of measuring the physical properties such as strength, thickness and water consumption of the cement clinker mortar and setting time according to the national standard are shown in Table 5.
TABLE 5 physical Properties of Cement Clinker and mortar Strength
Example 3:
drying the five raw materials at 105 ℃ for 12h, and then preparing the following components in percentage by weight: 61.18 percent of limestone, 15.82 percent of bauxite, 10.12 percent of sandstone, 8.52 percent of desulfurized gypsum and 1.76 percent of red mud, weighing 5kg of raw materials, uniformly mixing, adding 0.6 percent of borax and 2 percent of calcium phosphate which account for the total weight percent of the mixed materials, and grinding the mixture in a vibration mill until the residue of a square hole with the size of 0.075mm is 5 percent, thus obtaining the powdery cement raw material. Adding 8% of water by mass into the powdery cement raw materials, uniformly stirring, putting into a tablet press, pressing into a wafer with the diameter of 235mm, and drying at 105 ℃ for 12h. And taking out the materials, putting the materials into a muffle furnace preheated to 900 ℃ for calcining for 30 minutes, then transferring the materials into an electric furnace at 1290 ℃ for heat preservation for 1 hour, taking out the materials, and rapidly cooling the materials to room temperature by using a fan.
Crushing the cooled cement clinker, and grinding the crushed cement clinker to a specific surface area of 400 +/-20 m by using a ball mill 2 Fineness of/kg. The chemical composition of the cement clinker and the mineral composition of the clinker determined by the XRD diffraction quantitative analysis method are shown in Table 6.
TABLE 6 mineral composition of cement clinker
According to the national standard, the measurement results of the physical properties of the cement clinker mortar such as strength, standard consistency, water consumption, setting time and the like are shown in Table 7.
TABLE 7 physical Properties of Cement Clinker and mortar Strength
Comparative example 4
Drying the five raw materials at 105 ℃ for 12h, and then preparing the following components in percentage by weight: 61.18 percent of limestone, 15.87 percent of bauxite, 10.12 percent of sandstone, 11.07 percent of desulfurized gypsum and 1.76 percent of red mud, weighing 5kg of raw materials, uniformly mixing, and grinding in a vibration mill to obtain a powder cement raw material with 5 percent of square-hole screen residue of 0.075 mm. Adding 8% of water by mass into the powdery cement raw materials, uniformly stirring, putting into a tabletting machine, pressing into round pieces with the diameter of 235mm, and drying at 105 ℃ for 12h. The materials are taken out and put into a muffle furnace which is preheated to 900 ℃ for calcining for 30 minutes, then the muffle furnace is transferred to an electric furnace of 1290 ℃ for heat preservation for 1 hour, and the materials are taken out and rapidly cooled to the room temperature by a fan.
Crushing the cooled cement clinker, and grinding the crushed cement clinker to a specific surface area of 400 +/-20 m by using a ball mill 2 Fineness of/kg. The chemical composition of the cement clinker and the mineral composition of the clinker determined by the XRD diffraction quantitative analysis method are shown in Table 6.
TABLE 6 mineral composition of cement clinker
According to the national standard, the measurement results of the physical properties of the cement clinker mortar such as strength, standard consistency, water consumption, setting time and the like are shown in Table 7.
TABLE 7 physical Properties of Cement Clinker and mortar Strength
Compared with the case that 0.3-0.6% of borax and 1-2% of calcium phosphate are added into raw materials in the embodiment 1-3, the sintering condition of the clinker without adding boron and phosphorus in the embodiment 4 can be seen, and the flexural strength and the compressive strength of clinker mortar are obviously improved under the condition that the specific surface areas of the clinker are similar, which indicates that under the boron-phosphorus composite doping action, the sintering process of the clinker is advanced towards the direction of higher strength in the middle and later periods, and the boron-phosphorus composite doping can effectively improve the strength of the clinker in the middle and later periods.
Claims (3)
1. The boron-phosphorus composite modified high belite sulphoaluminate cement clinker is characterized in that the cement clinker comprises the following raw materials in percentage by mass: 55 to 70 percent of limestone, 12 to 20 percent of sandstone, 0 to 5 percent of Bayer process red mud, 5 to 15 percent of desulfurized gypsum, 5 to 15 percent of bauxite, 0.01 to 1 percent of borax and 0.01 to 2 percent of calcium phosphate.
2. The boron-phosphorus composite modified high belite sulphoaluminate cement clinker according to claim 1, wherein the minerals in the cement clinker comprise, in mass fraction percent: c 4 A 3 $:15%～30%,C 2 $:55%～75%,C 4 5 to 10 percent of AF, 5 to 20 percent of C and the balance of mixed mineral components.
3. The preparation method of the boron-phosphorus composite modified high belite sulphoaluminate cement clinker is characterized by comprising the following steps of:
(1) Pretreatment of raw materials:
drying the raw materials at 105 ℃ for 24 hours respectively, and crushing and grinding the raw materials by using a crusher until the 0.08mm screen residue is less than 8%;
(2) Premixing raw materials:
mixing 55-70% of limestone, 12-20% of sandstone, 0-5% of Bayer process red mud, 5-15% of desulfurized gypsum, 5-15% of bauxite, 0.01-1% of borax and 0.01-2% of calcium phosphate in a mixing tank, and then mixing in a mixer for 9 hours to obtain raw materials;
(3) Tabletting:
adding ultrapure water with the mass fraction of 8% into the premixed raw material, tabletting, and drying at 105 ℃ for 12 hours to obtain a dried raw material test block;
(4) Calcining clinker:
placing the raw material block prepared in the step (3) into a muffle furnace for calcining, raising the temperature to 900 ℃ at the heating rate of 5-10 ℃/min, and preserving the temperature for 0.5-1 h; then quickly transferring the test block to an environment of 1250-1350 ℃ and preserving the heat for 1h; and removing clinker after the calcination and quenching to obtain the high belite sulphoaluminate cement clinker.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116730638A (en) * | 2023-06-15 | 2023-09-12 | 济南大学 | Alkali-resistant iron-rich sulphoaluminate cement composite cementing material and preparation process thereof |
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| CN103964713A (en) * | 2014-05-21 | 2014-08-06 | 桂林理工大学 | Method for preparing belite-sulphate aluminium cement by using coal ashes and bayer-process red mud |
| CN108658485A (en) * | 2018-07-09 | 2018-10-16 | 深圳大学 | A kind of hydraulic cement clinker and preparation method thereof, hydraulic cement and its application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116730638A (en) * | 2023-06-15 | 2023-09-12 | 济南大学 | Alkali-resistant iron-rich sulphoaluminate cement composite cementing material and preparation process thereof |
| CN116730638B (en) * | 2023-06-15 | 2023-12-29 | 济南大学 | Alkali-resistant iron-rich sulphoaluminate cement composite cementing material and preparation process thereof |
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