CN110981259B - Additive for improving crystallinity of hydro-thermal synthesis hydrated calcium silicate - Google Patents
Additive for improving crystallinity of hydro-thermal synthesis hydrated calcium silicate Download PDFInfo
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- CN110981259B CN110981259B CN201911292983.XA CN201911292983A CN110981259B CN 110981259 B CN110981259 B CN 110981259B CN 201911292983 A CN201911292983 A CN 201911292983A CN 110981259 B CN110981259 B CN 110981259B
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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
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/18—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing mixtures of the silica-lime type
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/34—Non-shrinking or non-cracking materials
- C04B2111/343—Crack resistant materials
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/40—Porous or lightweight materials
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Abstract
The invention discloses an additive for improving the crystallinity of hydro-thermal synthesis hydrated calcium silicate, belonging to the field of new building materials. The hydrated calcium silicate modifier and the reinforcing agent are added into the silicate base material, so that the conversion of hydrated calcium silicate colloid to tobermorite crystals in the hydrothermal reaction process is accelerated, the hydro-thermally synthesized silicate base material is endowed with high strength and low shrinkage, and the hydro-thermally synthesized silicate aerated concrete material is suitable for improving the performance of hydro-thermally synthesized silicate aerated concrete materials such as hydrated calcium silicate plates, concrete high-strength tubular piles, lime-cement-sand aerated concrete, lime-cement-fly ash aerated concrete, lime-cement-sand-fly ash aerated concrete and the like produced by a hydrothermal method.
Description
Technical Field
The invention belongs to the technical field of building materials, and particularly relates to an additive for improving the crystallinity of hydro-thermal synthesis hydrated calcium silicate.
Background
The hydrated calcium silicate (C-S-H) is CaO-SiO2-H2The sum of the three-element compounds in the O system is an amorphous substance generated by hydration of tricalcium silicate and dicalcium silicate, and the amount of the amorphous substance is about 65 percent of the amount of a portland cement hydration product. The hydrated calcium silicate gel and tobermorite crystal are important hydration products of the aerated concrete, and the hydration products of the aerated concrete which is not steamed and cured mainly comprise flaky calcium hydroxide, needle-bar-shaped ettringite, fibrous and reticular C-S-H gel and more pores; the aerated concrete hydration product steamed and cured at 1MPa takes foliated tobermorite and curly low-calcium hydrated calcium silicate as main materials, and the tobermorite has higher crystallization degree.
In calcium silicate hydrate products, the crystallinity of the calcium silicate hydrate is of great significance. When the crystallinity is low, the content of calcium silicate hydrate colloid in the product is high, the drying shrinkage is large, and the service life of the calcium silicate hydrate product is obviously influenced; when the crystallinity is larger, the colloid content of the calcium silicate hydrate is less, the system is lack of binding of a cementing material, and the strength is reduced, so that the crystallinity of the calcium silicate hydrate exists in an optimal region. In the actual production process, due to the limitation of reaction conditions, the content of calcium silicate hydrate gel is low, the conversion process of calcium silicate hydrate colloid to tobermorite crystal is limited, and the crystallinity of calcium silicate hydrate is low. From the current state of research and application, the crystallinity of the hydro-thermal synthesis hydrated calcium silicate product has a great promotion space, so that research on how to promote the transformation of hydrated calcium silicate crystals to tobermorite and improve the crystallinity of hydrated calcium silicate is needed, so as to further promote the hydro-thermal synthesis of the hydrated calcium silicate product.
The crystallinity of the hydrated calcium silicate is a key factor influencing the physical mechanical property, the volume stability and the durability of the hydrothermal synthetic silicate material. One of the important technical approaches for improving the performance of aerated concrete is to optimize the crystallinity of hydrated calcium silicate. Therefore, the method for improving the conversion of the calcium silicate hydrate colloid to tobermorite crystals in the hydrothermal reaction process is of great significance.
Disclosure of Invention
The invention aims to provide an additive for improving the crystallinity of hydro-thermal synthesis hydrated calcium silicate, which can promote the conversion of hydrated calcium silicate colloid to tobermorite crystal, improve the strength, effectively reduce the shrinkage and reduce the shrinkage cracking of products.
In order to achieve the purpose, the invention adopts the following technical scheme:
an additive for improving the crystallinity of hydrothermal synthesis hydrated calcium silicate comprises a hydrated calcium silicate modifier and an enhancer;
the hydrated calcium silicate modifier is hydrated aluminosilicate and/or hydrated sulphoaluminate;
the intensifier is a mixture consisting of mirabilite and one or more of sodium metasilicate, sodium aluminate, sodium citrate or potassium sodium tartrate.
Further, the hydrated aluminosilicate is prepared by the following method: uniformly stirring sodium carbonate, metakaolin and water according to the weight ratio of 1:11.5:4.5 to prepare spherical particles with the diameter of less than 10mm, watering, naturally curing for 7 days, and crushing into particles with the diameter of less than 1 mm.
Further, the hydrated sulphoaluminate is prepared by adopting the following method: uniformly stirring anhydrous calcium sulphoaluminate clinker, gypsum, slaked lime and water according to the weight ratio of 1:2.2:0.8:2.2 to prepare spherical particles with the diameter of less than 10mm, watering, naturally curing for 14 days, and crushing into particles with the diameter of less than 1 mm.
Further, the weight of the mirabilite in the reinforcing agent accounts for 30-70% of the total weight of the reinforcing agent, and preferably 45-50%.
The additive is applied to hydrothermal synthesis of calcium silicate hydrate.
Furthermore, the application is that calcium silicate hydrate modifier, reinforcing agent and silicate base material are mixed and then are prepared into calcium silicate hydrate by conventional hydrothermal synthesis;
wherein, the dosage of the hydrated calcium silicate modifier, the reinforcing agent and the silicate base material is 85 to 95 percent of the silicate base material, 3 to 10 percent of the hydrated calcium silicate modifier and 2 to 5 percent of the reinforcing agent according to the mass percentage, and the sum of the mass percentages of all the raw materials is 100 percent.
Further, the silicate base material is a hydro-thermal synthesis silicate aerated concrete material selected from hydrated calcium silicate boards, concrete high-strength tubular piles, lime-cement-sand aerated concrete, lime-cement-fly ash aerated concrete and lime-cement-sand-fly ash aerated concrete.
According to the invention, the calcium silicate hydrate modifier and the reinforcing agent are added into the silicate base material, so that the conversion of calcium silicate hydrate colloid to tobermorite crystal in the hydrothermal reaction process is accelerated, the crystallinity of the hydrothermally synthesized calcium silicate hydrate is improved, the hydrothermally synthesized silicate base material is endowed with high strength and low shrinkage, and the method is suitable for improving the performance of hydrothermally synthesized silicate aerated concrete materials such as a hydrated calcium silicate plate, a concrete high-strength tubular pile, lime-cement-sand aerated concrete, lime-cement-fly ash aerated concrete, lime-cement-sand-fly ash aerated concrete and the like produced by a hydrothermal method.
Has the advantages that:
1. the monothio-type hydrated sulphoaluminate provides a source of aluminum-doped elements required by the aluminum-doped hydrated calcium silicate, thereby improving the chain length and the mechanical property.
2. Promote the formation of colloid, accelerate the transformation of colloid to tobermorite crystal, and obviously improve and strengthen the strength of concrete products. But simultaneously reduces the shrinkage, effectively prevents the cracking of products, building walls and the like, and has important significance for developing high-performance low-density, low-shrinkage and low-heat-conduction aerated concrete.
Drawings
Fig. 1 is XRD patterns of the test group 2 and the comparative group 1 in example 1.
Detailed Description
The following examples further illustrate the present invention but are not to be construed as limiting the invention. Modifications or substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit and scope of the invention. The experimental methods and reagents of the formulations not specified in the examples are in accordance with the conventional conditions in the art.
Mirabilite in the following examples is a salt chemical byproduct.
Example 1
In the embodiment, lime-cement-sand aerated concrete is used as a basic component of the silicate base material, and the raw material formulas of the test groups 1-3 and the comparative group 1 are shown in the following table:
in the above table:
modifying agentaIs one or two mixtures of hydrated aluminosilicate and hydrated sulphoaluminate;
reinforcing agentbIs prepared from mirabilite and its mixture with sodium metasilicate, sodium aluminate, sodium citrate and tartaric acidOne or a mixture of two or more of potassium and sodium acid;
common sandcThe content of the silicon dioxide is more than or equal to 68 percent;
cementdThe mark is PO42.5, and the content of calcium oxide is 70 percent;
quick limeeThe content of calcium oxide is more than 80 percent.
Mixing the hydrated calcium silicate modifier, the reinforcing agent and the silicate base material basic components in the test groups 1-3 and the comparison group 1 in proportion, uniformly stirring to obtain high-strength low-shrinkage silicate base material slurry, and mixing and stirring the foaming component and the high-strength low-shrinkage silicate base material slurry to obtain foam slurry; pouring the slurry into a mold for molding, curing for 3-7 hours at 40-50 ℃, and then removing the mold; and (3) removing the mould, cutting the formed product into building blocks with designed sizes, curing the building blocks for 6 to 10 hours under the autoclaved conditions of 1.1 to 1.5MPa and 175 to 185 ℃, and taking the building blocks out of a kettle to obtain the following measured strength and crystallinity of the lime-cement-sand aerated concrete:
as can be seen from the above table, the calcium silicate hydrate product prepared by the comparative group 1 has lower strength and crystallinity even under the same preparation process conditions because the calcium silicate hydrate modifier and the reinforcing agent are not added in the raw material composition. The calcium silicate hydrate products prepared by the test groups 1, 2 and 3 have different strength and crystallinity on the basis of different types of the added calcium silicate hydrate modifiers and reinforcing agents, and when the hydrated aluminosilicate is added as the calcium silicate hydrate modifier and the mirabilite, the sodium citrate and the potassium sodium tartrate are added as the reinforcing agents, the strength and the crystallinity of the products are highest. Compared with the comparison group 1, the hydrated calcium silicate products prepared by the test groups 1, 2 and 3 have greatly improved strength and crystallinity.
In the embodiment, SiO is excited by adding a hydrated calcium silicate modifier and a reinforcing agent2Active, increasing active SiO2The quantity of the modifier can play a role of crystal nucleus to promote the reaction furtherMore tobermorite is generated, and the strength of the lime-cement-sand aerated concrete product is obviously improved and enhanced.
FIG. 1 is XRD patterns of test group 2 and comparative group 1, wherein the XRD patterns are respectively lime-cement-sand aerated concrete (test group 2) doped with a hydrated calcium silicate modifier and a reinforcing agent, the XRD patterns are respectively shown as comparative group 1, Q is quartz, T is tobermorite, and P is calcium hydroxide. The results show that the test group 2 and the comparative group 1 contain portlandite and both contain distinct characteristic peaks of calcium silicate hydrate and tobermorite. Compared with the comparative group 1, the calcium silicate hydrate in the test group 2 has a sharper peak shape, has better crystallization performance and contains more tobermorite crystals. It was also confirmed in the calculation that the crystallinity of calcium silicate hydrate of test group 2 and comparative group 1 was 37.1 (wt.%) and 21 (wt.%), respectively, and the incorporation of the modifier and the enhancer of calcium silicate hydrate could excite SiO2Active, increasing active SiO2And meanwhile, the calcium silicate hydrate modifier plays a role of a crystal nucleus, promotes the reaction to further proceed, generates more tobermorite and obviously improves and enhances the crystallinity of a calcium silicate hydrate product.
Example 2
In the embodiment, lime-cement-fly ash aerated concrete is used as a basic component of the silicate base material, and the raw material formulas of the test groups 4-6 and the comparative group 2 are shown in the following table:
in the above table:
modifying agentaIs one or two mixtures of hydrated aluminosilicate and hydrated sulphoaluminate;
reinforcing agentbIs mixture of mirabilite and one or two or more of sodium metasilicate, sodium aluminate, sodium citrate and potassium sodium tartrate;
cementcThe mark is PO42.5, and the content of calcium oxide is 70 percent;
quick limedThe content of calcium oxide is more than 80 percent.
Mixing the hydrated calcium silicate modifier, the reinforcing agent and the silicate base material basic components in the test groups 4-6 and the comparison group 2 in proportion, uniformly stirring to obtain high-strength low-shrinkage silicate base material slurry, and mixing and stirring the foaming component and the high-strength low-shrinkage silicate base material slurry to obtain foam slurry; pouring the slurry into a mold for molding, curing for 3-7 hours at 40-50 ℃, and then removing the mold; and (3) removing the mould, cutting the formed product into building blocks with designed sizes, curing the building blocks for 6 to 10 hours under the autoclaved conditions of 1.1 to 1.5MPa and 175 to 185 ℃, and taking the building blocks out of a kettle to obtain the following measured strength and crystallinity of the lime-cement-fly ash aerated concrete:
as can be seen from the above table, the calcium silicate hydrate product prepared by the comparative group 2 has lower strength and crystallinity even under the same preparation process conditions because the calcium silicate hydrate modifier and the reinforcing agent are not added in the raw material composition. The calcium silicate hydrate products prepared by the test groups 4, 5 and 6 have greatly improved strength and crystallinity.
In the embodiment, SiO is excited by adding a hydrated calcium silicate modifier and a reinforcing agent2Active, increasing active SiO2And meanwhile, the calcium silicate hydrate modifier plays a role of a crystal nucleus, promotes the reaction to further proceed, generates more tobermorite and obviously improves and enhances the strength of the lime-cement-fly ash aerated concrete product.
Example 3
In the embodiment, lime-cement-sand-fly ash aerated concrete is used as a basic component of the silicate base material, and the raw material formulas of the test groups 7-9 and the comparative group 3 are shown in the following table:
in the above table:
modifying agentaIs one or two of hydrated aluminosilicate and hydrated sulphoaluminateMixing;
reinforcing agentbIs mixture of mirabilite and one or two or more of sodium metasilicate, sodium aluminate, sodium citrate and potassium sodium tartrate;
common sandcThe content of the silicon dioxide is more than or equal to 68 percent;
cementdThe mark is PO42.5, and the content of calcium oxide is 70 percent;
quick limeeThe content of calcium oxide is more than 80 percent.
Mixing hydrated calcium silicate modifier, reinforcing agent and silicate base material basic components in the test groups 7-9 and the comparison group 3 in proportion, uniformly stirring to obtain high-strength low-shrinkage silicate base material slurry, and mixing and stirring the foaming component and the high-strength low-shrinkage silicate base material slurry to obtain foam slurry; pouring the slurry into a mold for molding, curing for 3-7 hours at 40-50 ℃, and then removing the mold; and (3) removing the mould, cutting the obtained product into building blocks with designed sizes, curing the building blocks for 6 to 10 hours under the autoclaved conditions of 1.1 to 1.5MPa and 175 to 185 ℃, and taking the building blocks out of a kettle to obtain the following measured strength and crystallinity of the lime-cement-sand-fly ash aerated concrete:
as can be seen from the above table, the calcium silicate hydrate product prepared by the comparative group 3 has lower strength and crystallinity even under the same preparation process conditions because the calcium silicate hydrate modifier and the reinforcing agent are not added in the raw material composition. Test groups 7, 8 and 9 were doped with a calcium silicate hydrate modifier and a reinforcing agent to excite SiO2Active, increasing active SiO2And meanwhile, the calcium silicate hydrate modifier plays a role of a crystal nucleus, promotes the reaction to further proceed, generates more tobermorite and obviously improves and enhances the strength of the lime-cement-fly ash aerated concrete product.
Example 4
Two sets of hydrated calcium silicate plates of different compositions were selected for comparison in this example. The raw material composition of test set 10 was: 35-60% of quartz sand powder, 10-20% of slaked lime powder, 5-10% of fly ash and 10-20% of accelerating binder; the test group 11 is additionally added with 5 to 10 percent of calcium silicate hydrate modifier and 2 to 5 percent of reinforcing agent on the basis of the test group 10.
And uniformly stirring the two groups of materials in proportion, adding water to prepare slurry, molding, curing for 3-7 hours at 40-50 ℃, removing the mold, conveying the plate stack into an autoclave with the autoclave curing temperature of 160-180 ℃ and the pressure of 1.0-1.2 MPa for autoclave curing for 13-20 hours, and measuring the crystallinity of the hydrated calcium silicate plate after the plate stack is taken out of the autoclave.
Example 5
In this embodiment, two groups of concrete high-strength pipe piles with different components are selected as a comparison, and the raw materials of the test group 12 are as follows: 500-520 parts of PII 52.5 cement, 690-700 parts of sand, 1100-1200 parts of broken stone, 130-140 parts of water and 4-6 parts of a polycarboxylic acid water reducing agent; in test group 13, 45 to 80 parts of a hydrated calcium silicate modifier and 20 to 30 parts of a reinforcing agent are additionally added on the basis of test group 12.
Weighing the two groups of materials according to a certain proportion, respectively putting the materials into a stirrer, pre-stirring for 30s, adding water for stirring, uniformly and continuously pouring the stirred materials layer by layer from one end of a pipe pile die after stirring, then centrifugally forming, and finally maintaining.
The curing is normal pressure steam curing for 4 to 8 hours at 70 to 90 ℃ and high temperature and high pressure steam curing for 6 to 12 hours in an autoclave at 170 to 200 ℃.
Heating in an autoclave for 2h, keeping the temperature for 4h, cooling for 3h, standing for 1h, discharging the product out of the autoclave, and measuring the strength and the crystallinity of the concrete high-strength tubular pile after discharging the product out of the autoclave.
The properties of the articles obtained in example 4 and example 5 are as follows:
from the above table, it can be known that whether the hydrated calcium silicate plate or the concrete high-strength tubular pile product is added, the crystallinity of the hydrated calcium silicate can be obviously improved by adding the hydrated calcium silicate modifier and the reinforcing agent. Test groups 11, 13 incorporateHydrated calcium silicate modifier and enhancer for exciting SiO2Active, increasing active SiO2And meanwhile, the calcium silicate hydrate modifier plays a role of a crystal nucleus, promotes the reaction to further proceed, generates more tobermorite and obviously improves and enhances the crystallinity of a calcium silicate hydrate plate and a concrete high-strength tubular pile product.
Claims (4)
1. An additive for improving the crystallinity of hydro-thermal synthesis hydrated calcium silicate is characterized in that: comprises a hydrated calcium silicate modifier and a reinforcing agent;
the hydrated calcium silicate modifier is hydrated aluminosilicate and/or hydrated sulphoaluminate;
the reinforcing agent is a mixture consisting of mirabilite and one or more of sodium metasilicate, sodium aluminate, sodium citrate or potassium sodium tartrate;
the hydrated aluminosilicate is prepared by the following method: uniformly stirring sodium carbonate, metakaolin and water according to the weight ratio of 1:11.5:4.5 to prepare spherical particles with the diameter of less than 10mm, watering, naturally curing for 7 days, and crushing into particles with the diameter of less than 1 mm;
the hydrated sulphoaluminate is prepared by the following method: uniformly stirring anhydrous calcium sulphoaluminate clinker, gypsum, slaked lime and water according to the weight ratio of 1:2.2:0.8:2.2 to prepare spherical particles with the diameter of less than 10mm, watering, naturally curing for 14 days, and crushing into particles with the diameter of less than 1 mm.
2. The admixture of claim 1, wherein: the weight of the mirabilite in the reinforcing agent accounts for 30-70% of the total weight of the reinforcing agent.
3. Use of the admixture of claim 1 in the hydrothermal synthesis of hydrated calcium silicate.
4. Use according to claim 3, characterized in that: mixing a calcium silicate hydrate modifier, a reinforcing agent and a silicate base material, and preparing calcium silicate hydrate by conventional hydrothermal synthesis;
wherein, the consumption of the hydrated calcium silicate modifier, the reinforcing agent and the silicate base material is 85-95% of the silicate base material, 3-10% of the hydrated calcium silicate modifier and 2-5% of the reinforcing agent by mass percent, and the sum of the mass percent of all the raw materials is 100%;
the silicate base material is selected from hydrated calcium silicate plates, concrete high-strength tubular piles, lime-cement-sand aerated concrete, lime-cement-fly ash aerated concrete or lime-cement-sand-fly ash aerated concrete.
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CN114292043B (en) * | 2021-12-22 | 2023-03-17 | 江苏博拓新型建筑材料股份有限公司 | Tolbecco-mullite seed crystal inducer and preparation method thereof, aerated concrete prepared from inducer and preparation method of aerated concrete |
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