CN107056110B - metakaolin-based ordinary silicate cement mortar reinforcing agent and preparation method thereof - Google Patents
metakaolin-based ordinary silicate cement mortar reinforcing agent and preparation method thereof Download PDFInfo
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- CN107056110B CN107056110B CN201710212520.2A CN201710212520A CN107056110B CN 107056110 B CN107056110 B CN 107056110B CN 201710212520 A CN201710212520 A CN 201710212520A CN 107056110 B CN107056110 B CN 107056110B
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- metakaolin
- 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
- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/38—Fibrous materials; Whiskers
- C04B14/383—Whiskers
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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
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/02—Treatment
- C04B20/04—Heat treatment
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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
- 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
Abstract
The invention relates to metakaolin-based ordinary silicate cement mortar reinforcing agent and a preparation method thereof, wherein the reinforcing agent is obtained by mixing metakaolin and modified active fibers according to the mass ratio of 5:1-3, the modified active fibers are obtained by calcining dried and ball-milled phosphogypsum and then carrying out hydrothermal reaction, and phosphogypsum whiskers are obtained by calcining the phosphogypsum whiskers again, the metakaolin is put into a mixer, then the modified active fibers are added for mixing for 30-90min, and the metakaolin-based ordinary silicate cement mortar reinforcing agent is obtained after the mixing.
Description
Technical Field
The invention belongs to the technical field of building materials, and particularly relates to metakaolin-based ordinary silicate cement mortar reinforcing agents and a preparation method thereof.
Background
The concrete is the most widely applied building engineering material at present, and the main application fields are roads, bridges, water conservancy and hydropower, industry, civil buildings, military engineering and the like, because of the design defects of the concrete, the influence of factors such as environment and the like, part of the concrete can generate corrosion, alkali aggregate reaction, freeze-thaw damage and even cracks, and the stability and the safety of the structure are seriously influenced, so that the improvement of the strength of the concrete and the improvement of the durability of the concrete are key points and hot points of research.
The metakaolin is inorganic materials rich in active silicon-aluminum minerals, is prepared by calcining ball-milled kaolin at a proper temperature (500 ℃ C. and 800 ℃ C.) and then dehydrating, has very strong pozzolan activity, and can be used for preparing a concrete material with high compactness, high strength, excellent durability and excellent corrosion resistance.
Disclosure of Invention
The invention aims to solve the technical problem of providing metakaolin-based ordinary silicate cement mortar reinforcing agents and a preparation method thereof aiming at the defects in the prior art, wherein the reinforcing agents can effectively stimulate the pozzolanic activity of metakaolin in cement-based materials, greatly improve the early strength and the later strength of cement mortar, improve the surface bleeding phenomenon of the cement mortar, reduce the setting time, improve the fluidity, enhance the toughness of hardened cement mortar and have better improvement effect on the durability of cement concrete.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
providing metakaolin-based ordinary silicate cement mortar reinforcing agents, wherein the reinforcing agents are obtained by mixing metakaolin and modified active fibers according to the mass ratio of 5: 1-3;
the modified active fiber is prepared by calcining the dried and ball-milled phosphogypsum, performing hydrothermal reaction on the calcined phosphogypsum to obtain phosphogypsum whiskers, and calcining the phosphogypsum whiskers again to obtain the modified active fiber.
According to the scheme, the metakaolin is obtained by ball milling the metakaolin for 1-3 hours by a ball mill and calcining the metakaolin for 1-5 hours at the temperature of 500-800 ℃.
According to the scheme, the length-diameter ratio of the modified active fiber is 30-90, and the preparation method comprises the following steps:
1) drying the phosphogypsum at 40-60 ℃, then ball-milling and sieving by a 400-mesh sieve, wherein the screen residue is less than 1%, and then calcining for 2h at 550 +/-50 ℃ to obtain calcined phosphogypsum;
2) placing the calcined phosphogypsum obtained in the step 1) into a hydrothermal reaction kettle, and adding a mixed solution according to a solid-liquid mass ratio of 1:10-20, wherein the mixed solution is prepared by mixing glycerol and deionized water according to a volume ratio of 0.4-0.6: 1, carrying out hydrothermal reaction at the temperature of 120-160 ℃ for 1-3h, and centrifugally washing and drying the obtained product to obtain the phosphogypsum whisker;
3) calcining the phosphogypsum whisker obtained in the step 2) at the temperature of 200-600 ℃ for 3h to obtain the modified active fiber.
The phosphogypsum whiskers prepared by a hydrothermal method are usually calcium sulfate hemihydrate whiskers, are easy to absorb moisture in air and water to form dihydrate gypsum, and damage to a crystal structure is caused, so that modification treatment is required before application2+、SO4 2-Under the alkaline condition of a cement system, the cement mortar can react with active silicon-aluminum substances in metakaolin so as to excite the volcanic ash activity of the metakaolin, improve the hydration process and the structure of cement stone, enhance the early flexural strength of hardened cement mortar and improve the compressive strength of the hardened cement mortar; meanwhile, the anhydrous dead burned gypsum in the modified phosphogypsum whisker can also exert the micro-fiber characteristic of the phosphogypsum whisker and has the effects of enhancing and toughening hardened cement mortar.
The invention also provides a preparation method of the metakaolin-based ordinary silicate cement mortar reinforcing agent, which comprises the following steps: weighing metakaolin and modified active fiber in proportion, firstly putting metakaolin into a mixer, then adding the modified active fiber for mixing for 30-90min, and obtaining the metakaolin-based ordinary silicate cement mortar reinforcing agent after mixing.
The invention also provides the application of the metakaolin-based ordinary silicate cement mortar reinforcing agent in ordinary silicate cement mortar, wherein the mixing amount of the reinforcing agent is 6-8%.
Under the mechanical action, the reinforcing agent modified active fiber is adsorbed on the surface of the metakaolin through physical action and chemical action and enters the gaps of agglomerated metakaolin particles, and the modified active fiber has two functions of fully dispersing the agglomerated metakaolin and modifying the surface of the metakaolin particles through .
The invention has the beneficial effects that 1, the reinforcing agent prepared by the invention can obviously improve the early strength and the later strength of the ordinary silicate cement mortar, the mixing amount of the metakaolin-based ordinary silicate cement reinforcing agent in the ordinary silicate mortar is 6-8 wt%, the 3d flexural strength of the mortar can be obviously improved by more than 40%, the 7d flexural strength of the mortar can be obviously improved by more than 15%, and the 28d flexural strength growth rate can still be kept at more than 20%, the 3d compressive strength of the mortar can be obviously improved by more than 60%, the 7d compressive strength of the mortar can be obviously improved by more than 45%, and the 28d compressive strength growth rate can still be kept at more than 25%, because metakaolin is used as mineral admixtures, the metakaolin has the pozzolan activity and the micro-filling effect, the early strength and the later durability of the concrete can be obviously improved, and meanwhile, the active fiber in the metakaolin plays a good modifying effect and greatly stimulates the activity of the metakaolin;
2. the metakaolin-based ordinary portland cement reinforcing agent utilizes the combined action of metakaolin and calcined phosphogypsum whiskers to play the role of enhancing and toughening metakaolin and pozzolan activity and phosphogypsum whisker microfine fiber, and the metakaolin has higher specific surface area and fineness, has pozzolan effect and micro-filling effect, and can improve the water retention property of concrete mixture after being mixed so as to increase the coagulation property of cement mortarActive fiber mixed with crystal whisker and anhydrous dead burned gypsum crystal whisker. The anhydrous dead-burned gypsum whisker has larger atomic accumulation, no channel exists in crystal lattices, the crystal structure is firmer, almost no hydration occurs, the fiber characteristic can be exerted, and the breaking strength of hardened cement slurry is increased; while the crystal lattice of the anhydrous soluble gypsum whisker is neutralized with Ca2+‐SO4 2‐‐Ca2+The channels parallel to the chains are in a completely dehydrated state, have large specific surface area, can strongly absorb water when meeting water, firstly form calcium sulfate hemihydrate whiskers, and then are further hydrated by steps to generate SO4 2‐And the exciting effect of the sulfate on the activity of the metakaolin is exerted. Therefore, the flexural strength and compressive strength of the hardened cement mortar at various ages can be improved. When the metakaolin and the phosphogypsum whiskers are fully mixed, the activity of the metakaolin is greatly excited, so that the common silicate cement mortar has better working performance;
3. the invention can improve the volume stability and durability of the common silicate cement mortar, and after metakaolin is added into the common silicate cement mortar, the compactness of the product can be improved due to the volcanic ash effect and the micro-filling effect of the metakaolin, thereby effectively reducing the volume shrinkage and improving the durability of concrete. The addition of the metakaolin-based ordinary silicate cement mortar reinforcing agent improves the working performance of the ordinary silicate cement mortar, improves the reaction activity of metakaolin, and is more favorable for reducing the volume shrinkage of the ordinary silicate cement mortar and improving the durability of the ordinary silicate cement mortar.
Drawings
FIG. 1 is a comparative graph of flexural strength of a reference sample, a metakaolin sample and mortar test pieces of examples 1, 2 and 3, which are prepared by the method of the invention;
FIG. 2 is a graph comparing the compressive strength of the reference sample, the metakaolin sample and the mortar test pieces of examples 1, 2 and 3.
Detailed Description
In order to make the technical solution of the present invention better understood, the present invention is further described in detail with reference to the attached drawings.
The preparation method of the metakaolin used in the embodiment of the invention comprises the following steps: the kaolin is ball-milled for 2 hours by a ball mill and calcined for 3 hours at 800 ℃ to obtain metakaolin.
The preparation method of the modified active fiber comprises the following steps: drying raw material phosphogypsum at 45 ℃, performing ball milling in a ball mill for 1h, sieving with a 400-mesh sieve until the screen residue is less than 1%, calcining undersize products at 550 ℃ for 2h at the heating rate of 5 ℃/min, naturally cooling to obtain calcined phosphogypsum, then placing the calcined phosphogypsum in a hydrothermal reaction kettle, and adding a mixed solution according to the solid-liquid mass ratio of 1:20, wherein the mixed solution is prepared by mixing glycerol and deionized water according to the volume ratio of 0.5: 1, carrying out hydrothermal reaction for 2h at 140 ℃, centrifuging, washing and drying the obtained product to obtain the phosphogypsum whisker, wherein the length-diameter ratio of the whisker is 80.32, and the synthesis rate of the whisker is 93.40%, and the prepared phosphogypsum whisker is calcined for 3h at 200 ℃, 400 ℃ and 600 ℃ respectively to obtain a modified active fiber at 200 ℃, a modified active fiber at 400 ℃ and a modified active fiber at 600 ℃.
Example 1
The preparation method of the metakaolin-based ordinary silicate cement mortar reinforcing agent is characterized by comprising the following steps: putting the dried metakaolin into a mixer, adding 200 ℃ modified active fiber, and mixing for 30-90min to obtain the metakaolin-based ordinary silicate cement mortar reinforcing agent, wherein 5 parts of metakaolin are mixed with 1 part, 2 parts and 3 parts of modified active fiber respectively according to the mass parts to obtain three reinforcing agents (corresponding to 6%, 7% and 8% mixing amount).
The three prepared reinforcing agents respectively replace cement according to 6%, 7% and 8% of mixing amount (5% of metakaolin added with 1%, 2% and 3% of modified active fibers), standard sand is selected, and mortar test pieces with 6%, 7% and 8% of mixing amount are obtained according to the water-cement ratio of 0.5.
The preparation method of the metakaolin sample comprises the following steps: the metakaolin replaces cement with 5 percent of equivalent weight, selects standard sand and prepares mortar according to the water-cement ratio of 0.5.
The preparation method of the reference sample comprises the following steps: the cement mortar is prepared from 450g of ordinary Portland cement, 1350g of standard sand and 0.5 of water-cement ratio.
Testing the fluidity of the mixtures of the reference sample, the metakaolin sample and the reinforcing agent of the embodiment 1 according to GB/T2429-2005 'cement mortar fluidity testing method'; the flexural and compressive strengths of the reference samples and 3, 7 and 28 days of example 1 were tested using a universal pressure tester in accordance with GB/T17671-1999 Cement mortar Strength test method.
TABLE 1
Table 1 shows that compared with the metakaolin with the same doping amount of 5%, the fluidity of the mortar test piece in example 1 is improved by percent and can be improved to 195mm at most from 185mm, which shows that the metakaolin-based ordinary silicate cement mortar reinforcing agent prepared in the example has percent improvement effect on the working performance, compared with the reference sample and the metakaolin sample, the flexural strength and the compressive strength of the reinforcing agent doped in the example at all ages are improved, the flexural strength of 3d, 7d and 28d of the reference sample is respectively 5.5MPa, 8.2MPa and 9.1MPa, the compressive strength is respectively 22.3MPa, 37.6MPa and 46.4MPa, when the reinforcing agent doped in the example is added, the flexural strength of 3d, 7d and 28d can respectively reach 8.1MPa, 10.1MPa and 11.4MPa, the flexural strength of 3d, 7d and 28d can respectively improve by 47.27 percent, 23.17 percent and 25.27 percent, and the flexural strength of 3d, 7d and 28d can respectively reach 37.6MPa, 62 MPa, 62.58 MPa and 41.4 percent and 3644 percent.
The mixing amount of the reinforcing agent in this example was selected to be 7%, and the initial setting time and the final setting time of the reference sample (P.O42.5 cement), the metakaolin sample and the reinforcing agent in this example (all the mixing amounts were 7% by mass of the substituted cement) were measured by referring to the method for measuring the setting time of cement in GB/T1346-2001 "method for testing Water consumption, setting time and stability at Standard consistency of Cement".
TABLE 2
Table 2 shows that the metakaolin is added to shorten the initial setting time and the final setting time of the slurry correspondingly, meanwhile, the reinforcing agent prepared in the embodiment can further shorten the setting time of the cementing material by steps, wherein the initial setting time is shortened by 44min and the final setting time is shortened by 48min compared with a reference sample, which shows that the invention has fixed setting acceleration effect on concrete.
Example 2
The preparation method of the metakaolin-based ordinary silicate cement mortar reinforcing agent is characterized by comprising the following steps: putting the dried metakaolin into a mixer, adding 400 ℃ modified active fiber, and mixing for 30-90min to obtain the metakaolin-based ordinary silicate cement mortar reinforcing agent, wherein 5 parts of metakaolin are mixed with 1 part, 2 parts and 3 parts of modified active fiber respectively according to the mass parts to obtain three reinforcing agents (corresponding to 6%, 7% and 8% of mixing amount). When in use, the prepared reinforcing agent is used for replacing cement according to 6%, 7% and 8% of mixing amount (5% of metakaolin and 1%, 2% and 3% of modified active fibers), standard sand is selected, and mortar test pieces with 6%, 7% and 8% of mixing amount are obtained according to the water-cement ratio of 0.5.
The metakaolin sample and the reference sample were prepared in the same manner as in example 1.
The flexural strength and compressive strength of the reference sample and the 6%, 7%, 8% mortar test pieces of this example were measured by a universal pressure tester for 3 days, 7 days and 28 days in the same manner as in example 1.
TABLE 3
Table 3 shows that the fluidity of the mortar test piece in the embodiment is improved by percent compared with that of metakaolin with the same doping amount of 5 percent, and can be improved to 195mm at most from 185mm, which shows that the metakaolin-based ordinary silicate cement mortar reinforcing agent prepared in the embodiment has percent improvement effect on the working performance.
The mixing amount of the reinforcing agent prepared in this example was selected to be 7%, and the initial setting time and the final setting time of the standard sample (P.O42.5 cement), the metakaolin sample and the reinforcing agent of this example (all the mixing amounts were 7% by mass of the substituted cement) were measured by referring to the method for measuring the setting time of cement in GB/T1346-2001 "method for testing Water consumption, setting time and stability at Standard consistency of Cement".
TABLE 4
Table 4 shows that the metakaolin is added to shorten the initial setting time and the final setting time of the slurry correspondingly, meanwhile, the reinforcing agent added in the embodiment can further shorten the setting time of the cementing material by steps, wherein the initial setting time is shortened by 37min and the final setting time is shortened by 43min compared with a reference sample, which shows that the invention has fixed setting acceleration effect on concrete.
Example 3
The preparation method of the metakaolin-based ordinary silicate cement mortar reinforcing agent is characterized by comprising the following steps: putting the dried metakaolin into a mixer, adding 600 ℃ modified active fiber, and mixing for 30-90min to obtain the metakaolin-based ordinary silicate cement mortar reinforcing agent, wherein 5 parts of metakaolin are mixed with 1 part, 2 parts and 3 parts of modified active fiber respectively according to the mass parts to obtain three reinforcing agents (corresponding to 6%, 7% and 8% of mixing amount). When in use, the three prepared reinforcing agents respectively replace cement according to 6 percent, 7 percent and 8 percent of doping amount (5 percent of metakaolin and 1 percent, 2 percent and 3 percent of modified active fiber), standard sand is selected, and mortar test pieces with 6 percent, 7 percent and 8 percent of doping amount are obtained according to the water-cement ratio of 0.5.
The metakaolin sample and the reference sample were prepared in the same manner as in example 1.
The flexural strength and compressive strength of the reference sample and the 6%, 7%, 8% mortar test pieces of this example were measured by a universal pressure tester for 3 days, 7 days and 28 days in the same manner as in example 1.
TABLE 5
Table 5 shows that the fluidity of the mortar test piece in the embodiment is improved by percent compared with that of metakaolin with the same doping amount of 5 percent, and can be improved to 195mm at most from 185mm, which shows that the metakaolin-based ordinary silicate cement mortar reinforcing agent in the embodiment 3 has percent improvement effect on the working performance.
As shown in FIG. 1, which is a comparison graph of the flexural strength of the reference sample, the metakaolin sample and the mortar samples (7% of the reinforcing agent) prepared in examples 1, 2 and 3, it can be seen that the flexural strength of the metakaolin sample is improved in terms of 3d, 7d and 28d compared with the reference sample, and the flexural strength of the mortar samples is further improved in terms of after the reinforcing agent prepared in this example is added.
Fig. 2 is a comparison graph of the compressive strength of the reference sample and the metakaolin sample prepared by the invention and the mortar test pieces (the mixing amount of the reinforcing agent is 7%) in examples 1, 2 and 3, and it can be seen that the reinforcing agent prepared by the embodiment also has obvious improvement on the compressive strength of the mortar test pieces, and the improvement effect is better than metakaolin.
The mixing amount of the reinforcing agent in this example was selected to be 7%, and the initial setting time and the final setting time of the reference sample (P.O42.5 cement), the metakaolin sample and the reinforcing agent in this example (all the mixing amounts were 7% by mass of the substituted cement) were measured by referring to the method for measuring the setting time of cement in GB/T1346-2001 "method for testing Water consumption, setting time and stability at Standard consistency of Cement".
TABLE 6
Table 6 shows that the metakaolin is added to shorten the initial setting time and the final setting time of the slurry correspondingly, and meanwhile, the reinforcing agent added in the embodiment can further shorten the setting time of the cementing material by steps, wherein the initial setting time is shortened by 44min and the final setting time is shortened by 46min relative to a reference sample, which shows that the invention has fixed setting acceleration effect on concrete.
Claims (4)
1, metakaolin-based ordinary silicate cement mortar reinforcing agents, which are characterized in that the reinforcing agents are obtained by mixing metakaolin and modified active fibers according to the mass ratio of 5: 1-3;
the modified active fiber is prepared by calcining the dried and ball-milled phosphogypsum and then carrying out hydrothermal reaction on the calcined phosphogypsum to obtain phosphogypsum whiskers, and calcining the phosphogypsum whiskers again to obtain the modified active fiber;
the length-diameter ratio of the modified active fiber is 30-90, and the preparation method comprises the following steps:
1) drying the phosphogypsum at 40-60 ℃, then ball-milling and sieving by a 400-mesh sieve, wherein the screen residue is less than 1%, and then calcining for 2h at 550 +/-50 ℃ to obtain calcined phosphogypsum;
2) placing the calcined phosphogypsum obtained in the step 1) into a hydrothermal reaction kettle, and adding a mixed solution according to a solid-liquid mass ratio of 1:10-20, wherein the mixed solution is prepared by mixing glycerol and deionized water according to a volume ratio of 0.4-0.6: 1, carrying out hydrothermal reaction at the temperature of 120-160 ℃ for 1-3h, and centrifugally washing and drying the obtained product to obtain the phosphogypsum whisker;
3) calcining the phosphogypsum whisker obtained in the step 2) at the temperature of 200-600 ℃ for 3h to obtain the modified active fiber.
2. The metakaolin-based portland cement mortar reinforcing agent according to claim 1, wherein the metakaolin is obtained by ball milling of metakaolin through a ball mill for 1-3 hours and calcining at 500-.
3, A process for preparing the reinforcing agent of metakaolin-based ordinary silicate cement mortar as claimed in any of claims 1-2, which comprises the steps of proportioning metakaolin and modified active fibres, charging metakaolin into a mixer, charging modified active fibres, mixing for 30-90min, and mixing to obtain the reinforcing agent.
4. Use of metakaolin-based portland cement mortar reinforcing agent according to any one of claims 1-2 and , wherein the reinforcing agent is incorporated in an amount ranging from 6 to 8%.
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| CN107628790B (en) * | 2017-09-28 | 2020-04-24 | 嘉华特种水泥股份有限公司 | Decorative cement |
| CN107500674A (en) * | 2017-09-28 | 2017-12-22 | 嘉华特种水泥股份有限公司 | A kind of environment-friendly type decoration cement |
| CN108947414B (en) * | 2018-09-26 | 2020-07-28 | 济南大学 | High-compactness silicate cement mortar |
| CN115159910B (en) * | 2022-09-07 | 2022-12-06 | 广东潮泰建设有限公司 | Preparation method and application of high-strength waterproof concrete for building construction |
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