CN111499238A - Preparation method of zeolite geopolymer cementing material - Google Patents
Preparation method of zeolite geopolymer cementing material Download PDFInfo
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- CN111499238A CN111499238A CN202010559742.3A CN202010559742A CN111499238A CN 111499238 A CN111499238 A CN 111499238A CN 202010559742 A CN202010559742 A CN 202010559742A CN 111499238 A CN111499238 A CN 111499238A
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- zeolite
- geopolymer
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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
- C04B12/00—Cements not provided for in groups C04B7/00 - C04B11/00
- C04B12/005—Geopolymer cements, e.g. reaction products of aluminosilicates with alkali metal hydroxides or silicates
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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
- C04B7/24—Cements from oil shales, residues or waste other than slag
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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
- C04B7/24—Cements from oil shales, residues or waste other than slag
- C04B7/26—Cements from oil shales, residues or waste other than slag from raw materials containing flue dust, i.e. fly ash
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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
The invention discloses a preparation method of a zeolite geopolymer cementing material, which comprises the following steps: (1) preparing a silicon-aluminum mixture; (2) preparing an alkaline activating agent; (3) preparing zeolite geopolymer gelled material. The geopolymer cementing material reasonably utilizes raw materials such as metakaolin, zeolite, red mud, fly ash, magnesium oxide and the like, the activation reaction of each material component is promoted, alkali metal ions are firmly combined in a reaction product, and the problem of surface blooming can be slightly relieved. The zeolite geopolymer cementing material prepared by the invention has high strength and high hardening speed, and the strength can reach more than 48MPa in 28 days. The magnesium oxide in the raw material plays the role of a filling and expanding agent and can effectively absorb carbon dioxide. Through optimizing the proportion, the geopolymer has better corrosion resistance than common Portland cement, less capillary pores, good impermeability, small shrinkage, high condensation speed and strong applicability, and meets the sustainable development requirement of ecological environmental protection.
Description
Technical Field
The invention belongs to the field of building materials, and particularly relates to a zeolite geopolymer cementing material and a preparation method thereof.
Background
The geopolymer is prepared into a new material by the corresponding treatment and reaction of materials such as calcined clay (metakaolin), alkali excitant and the like. The inorganic polymer material with three-dimensional oxide network structure has the performance similar to that of ceramic and superior to that of cement. The materials in the manufacturing process do not need high-temperature treatment and can be directly used or used at low temperature, the raw materials are simple and have wide sources, the price is low, the emission of carbon dioxide is less than that of cement, and the energy is saved and the emission is reduced. Meanwhile, under the alkaline condition, the dehydration reaction of the geopolymeric aluminosilicate is reversible, and the product can be recycled after being crushed, so that the method is more environment-friendly than cement. The preparation process is simple, the crystal-like structure can wrap metal ions and toxic substances, the internal ions can also adsorb the metal ions, the gelling effect is very quick, and the high strength can be achieved in a short time. It is reported that geopolymer cement has a high strength retention rate even under acidic conditions, has high acid resistance, and has a slow strength decrease.
The CN105271848A is prepared by taking kaolin and manganese tailing slag as main raw materials, has simple preparation process, utilizes the manganese tailing slag to replace part of metakaolin, reduces the cost of geopolymer cementing materials, improves the comprehensive utilization degree of the manganese tailing, but hardly ensures the cementing effect of geopolymer due to the doping amount and modulus of alkali activator water glass, and has larger shrinkage.
The current geopolymer cements present mainly the following problems: (1) fast setting, how to control the setting time in a proper range without obviously reducing the strength; (2) the surface is easy to bloom, which not only affects the appearance of the product, but also reduces the impermeability of the product and the bonding strength between the interface and the interface; (3) the long-term process of alkali aggregate reaction destruction is very necessary for the deep research of various mineral admixtures or additives for inhibiting the alkali aggregate reaction; (4) shrinkage, wherein the shrinkage can be reduced by mastering the properties and the relationship among the components through corresponding means; (5) the strength is easy to fluctuate, the mineral structure is unstable, and the like, in addition, the activity of the fly ash is difficult to activate, the problems are controlled within a reasonable range, and the method has important significance for realizing the maximum utilization of substances and good use effect.
Disclosure of Invention
The invention mainly aims to provide a zeolite geopolymer cementing material which can meet the required strength after being hydrated for 6 hours at 20 ℃, has quick setting time and high strength, relieves the problem of surface blooming, achieves the effects of small shrinkage and good corrosion resistance, and can be applied to roads, bridges, military facilities and the like for quick rush repair aiming at the defects in the prior art.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a method of preparing a zeolitic geopolymer cement comprising the steps of:
1) preparing a silicon-aluminum mixture: a. washing, filtering and drying large blocks of pure fine kaolin, then putting the large blocks of pure fine kaolin into a stainless steel tank of a planetary ball mill for grinding for 3 hours, screening the large blocks of pure fine kaolin, putting the large blocks of pure fine kaolin into a high-temperature furnace, and calcining the large blocks of pure fine kaolin for 2 hours at 700 ℃ to obtain metakaolin powder; b. mixing a certain amount of fly ash, zeolite, magnesium oxide and red mud, uniformly mixing and drying to obtain a silicon-aluminum mixture;
2) preparing an alkaline activator: firstly, sodium hydroxide and a certain amount of water are melted to obtain a sodium hydroxide solution, then water glass is added to prepare alkali activity activators with different moduli, and the alkali activity activators are placed at normal temperature and cooled for 12 hours;
3) preparation of zeolitic geopolymer cement: slowly adding the silicon-aluminum mixture into an alkaline activator, adding distilled water while stirring until the liquid-solid ratio is 2/1, fully stirring, placing into an oven at 85 ℃, preserving for 12 hours, and demolding to obtain the zeolite geopolymer cementing material.
As a preferred technical solution of the present invention, the step 1) specifically includes: 100 parts of metakaolin, 10-15% of fly ash, 5-12% of zeolite, 1-5% of magnesium oxide and 10-15% of red mud, wherein the mass of the fly ash, the mass of the magnesium oxide and the mass of the red mud are respectively calculated according to the mass ratio of the metakaolin; the activity index of the metakaolin is more than or equal to 110.
As a preferred technical scheme of the invention, the fly ash adopts secondary fly ash, and the content of silicon dioxide is more than 45%; the zeolite is powder after grinding and screening, and the density is 2.27g/cm3The particle size is 100-120 meshes; the magnesium oxide is white amorphous powder, and the particle size of the magnesium oxide is less than 2 mu m; the red mud is prepared by adopting a ball millGrinding for 40min, grinding, and sieving to obtain powder with fineness greater than 31% and loss on ignition less than 7%; the materials are prepared into a silicon-aluminum mixture according to the proportion, and the silicon-aluminum mixture is taken as 100 parts.
As a preferable technical scheme of the invention, the alkaline activator in the step 2) is prepared from 190 parts of sodium hydroxide and 25-30 parts of water glass, the modulus of the water glass is 1.4, and the ratio of the sodium hydroxide to the effective component is more than 97%.
As a preferable technical scheme of the invention, the distilled water in the step 3) is added to meet the water-cement ratio of 0.35, the water-cement ratio is the mass percentage of the water and the silicon-aluminum mixture, and the water-cement ratio is water containing water glass and water generated by sodium hydroxide.
As a preferred technical scheme of the invention, the prepared zeolite geopolymer gelled material is wrapped on a component by a preservative film at 45 ℃ for 9 days of maintenance, and then natural maintenance is carried out.
Compared with the prior art, the invention has the following beneficial effects:
the aluminosilicate raw material is gradually polymerized into gel with high polymerization degree after being decomposed into aluminosilicate monomers under the alkaline condition, and finally, a zeolite-like structure substance is generated, and the substance is combined through ionic bonds and covalent bonds, has strong associativity, basically does not react with corrosive media, and has strong corrosion resistance. The zeolite is adopted, so that the internal pore structure of the material can be refined, the porosity is reduced, water is adsorbed and released, meanwhile, alkali metal ions in the material are adsorbed, alkali silicate reaction is inhibited, and volume shrinkage and microcracks are reduced; the magnesium oxide can play a remarkable role in cementing and filling in geopolymer, reacts with water to generate magnesium hydroxide, can absorb water in the environment of carbon dioxide to generate carbonized products, such as flaky hydrocarbonite and other substances, and also plays the roles of an expanding agent and a carbonation buffering agent, so that the carbonized products can also effectively absorb carbon dioxide, and the anti-carbonization performance of the geopolymer gelled material is improved; red mud and metakaolin form geopolymer under the effect of alkali activity excitant, internal aluminate and alkaline substances are consumed, the use of metakaolin is reduced, and the reasonable utilization of waste is realized; the mechanical property of geopolymer concrete can be improved by using the fly ash and the metakaolin, and the geopolymer cementing material overcomes the property change caused by dehydration and disintegration of crystals and dehydration of colloid.
The zeolite geopolymer cementing material obtained by the invention has high strength, quick hardening, no retarder and density of 2.3-2.7g/cm3The Mohs hardness is 5-6, the strength can reach 20MPa in 3 days, the capillary porosity is 17% -21%, the impermeability is good, the shrinkage is small, the reinforcing steel bar can be prevented from being corroded, the protective layer can not crack and peel greatly, the corrosion resistance is better than that of common cement, and the high strength can be maintained even if the cement is placed in seawater for a long time.
[ detailed description ] embodiments
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The alkali activity excitant is mixed liquid of sodium hydroxide and water glass, and the preparation process is as follows: firstly, sodium hydroxide and water are mixed to obtain sodium hydroxide solution, then water glass is added to prepare alkali activity excitants with different moduli. Wherein the sodium hydroxide is commercially available graded pure with purity of 97%, the water glass is commercially available industrial water glass with baume degree of 40%, and Na2The mass fraction of O is 8.98 percent and SiO is2The mass fraction is 29.23%.
EXAMPLE 1 preparation of Zeolite Geopolymer gelled Material
The fly ash used in the embodiment of the invention adopts secondary fly ash, and the content of silicon dioxide is 56%. Examples the preparation method is as follows:
1) preparing a silicon-aluminum mixture: a. washing, filtering and drying large blocks of pure fine kaolin, then putting the large blocks of pure fine kaolin into a stainless steel tank of a planetary ball mill for grinding for 3 hours, screening the large blocks of pure fine kaolin, putting the large blocks of pure fine kaolin into a high-temperature furnace, and calcining the large blocks of pure fine kaolin for 2 hours at 700 ℃ to obtain metakaolin powder; b. mixing a certain amount of fly ash, zeolite, magnesium oxide and red mud, uniformly mixing and drying to obtain a silicon-aluminum mixture, and taking 100 parts of the mixture;
2) preparing an alkaline activator: firstly, sodium hydroxide and a certain amount of water are melted to obtain a sodium hydroxide solution, then water glass is added to prepare an alkali activity excitant with the modulus of 1, and the alkali activity excitant is placed at normal temperature and cooled for 12 hours;
3) preparation of zeolitic geopolymer cement: slowly adding the silicon-aluminum mixture into an alkaline activator, adding distilled water while stirring until the liquid-solid ratio is 2/1, fully stirring, placing into an oven at 85 ℃, preserving for 12 hours, and demolding to obtain the zeolite geopolymer cementing material.
The preparation ratio of the silicon-aluminum raw material is as follows: 100 parts of metakaolin, 12 parts of fly ash, 10 parts of zeolite, 4 parts of magnesium oxide and 13 parts of red mud. The zeolite in the mixture is subjected to levigating screening treatment, and the red mud is also prepared by adopting treatment modes such as Bayer process high-temperature calcination, filter pressing and evaporation drying and the like.
Example 2 preparation of zeolitic geopolymer cement:
in the example, only the mixture ratio of the silicon-aluminum raw materials is different, and the mixture ratio of the silicon-aluminum raw materials comprises 100 parts of metakaolin, 12 parts of fly ash, 15 parts of zeolite, 4 parts of magnesium oxide and 15 parts of red mud.
Alkaline activator preparation and preparation of geopolymer cement the same as in example 1.
Comparative example 1 preparation of non-zeolitic geopolymer cement:
in the comparative example, zeolite is not doped, and the mixture ratio of the silicon-aluminum mixture is 100 parts of metakaolin, 12 parts of fly ash, 4 parts of magnesium oxide and 13 parts of red mud. The red mud is prepared by treatment modes such as Bayer process high-temperature calcination, filter pressing and evaporation to dryness.
Alkaline activator preparation and preparation of geopolymer cement the same as in example 1.
Comparative example 2 preparation of a geopolymer cement without zeolite and magnesium oxide:
in the comparative example, zeolite and magnesium oxide are not mixed, and the mixture ratio of the silicon-aluminum mixture is 100 parts of metakaolin, 12 parts of fly ash and 13 parts of red mud. The red mud is also prepared by treatment modes such as Bayer process high-temperature calcination, filter pressing and evaporation to dryness.
Comparative example the procedure was as follows:
1) preparing a silicon-aluminum mixture: a. washing, filtering and drying large blocks of pure fine kaolin, then putting the large blocks of pure fine kaolin into a stainless steel tank of a planetary ball mill for grinding for 3 hours, screening the large blocks of pure fine kaolin, putting the large blocks of pure fine kaolin into a high-temperature furnace, and calcining the large blocks of pure fine kaolin for 2 hours at 700 ℃ to obtain metakaolin powder; b. mixing a certain amount of fly ash and red mud, uniformly mixing and drying to obtain a silicon-aluminum mixture, and taking 100 parts;
2) preparing an alkaline activator: firstly, sodium hydroxide and a certain amount of water are melted to obtain a sodium hydroxide solution, then water glass is added to prepare an alkali activity excitant with the modulus of 1, and the alkali activity excitant is placed at normal temperature and cooled for 12 hours;
3) preparation of zeolitic geopolymer cement: slowly adding the silicon-aluminum mixture into an alkaline activator, adding distilled water while stirring until the liquid-solid ratio is 2/1, fully stirring, placing into an oven at 85 ℃, preserving for 12 hours, and demolding to obtain the zeolite geopolymer cementing material.
The samples of geopolymer gelled materials of examples 1-2 and comparative examples 1-2 were tested for compressive strength, shrinkage and corrosion resistance, and the zeolite geopolymer gelled materials prepared by the present invention were evaluated comprehensively by the following specific methods:
1. in the geopolymer cementing material strength test, referring to GB/T17671-1999 Cement mortar Strength detection method (ISO method), the raw materials are added into a cement mortar stirrer according to a pre-designed proportion and stirred uniformly, then the mixture is poured into a mold, molded by vibration, the size of the mold is 40mm × 40mm × 160mm, the mold is cured according to a corresponding mode, and the strength of the geopolymer cementing material is measured after 28 days.
2. Drying shrinkage test, namely performing a shrinkage test according to JC/T603-2004, wherein the size of the test piece is 40mm × 40mm 3540 mm × 160mm, testing the length of the test piece by using a calibrated comparator after curing for two days, and measuring the length of 28 days by using the test method as an initial value according to relevant regulations.
3. And (3) corrosion resistance test: the ratio of the compressive strength of the test piece after being soaked in the corrosive solution (acid corrosion resistance) to the compressive strength of the test piece after being maintained in water to the same age is taken as the corrosion resistance coefficient of the test piece, and the corrosion period is 60 days.
The concrete has the following performance results:
TABLE 1 basic Properties of zeolitic geopolymer cements in this connection
| Test of | Compressive strength (MPa) | Shrinkage rate (× 10)-6） | Corrosion resistance coefficient (%) |
| Example 1 | 48.2 | 175 | 94.8 |
| Example 2 | 43.9 | 189 | 90.3 |
| Comparative example 1 | 49.3 | 213 | 91.2 |
| Comparative example 2 | 45.6 | 255 | 89.8 |
The comparison results in Table 1 show that the cement prepared in examples 1-2 and comparative examples 1-2 had a smaller tendency to differ in compressive strength because the amount of zeolite and magnesium oxide incorporated was smaller and the gelling effect was not significantly affected, but it was found that the cement with zeolite and magnesium oxide added shrunk less than the cement without zeolite and magnesium oxide. The zeolite can consume alkalization decomposition energy in the reaction for accumulation, and the aluminosilicate mineral structure adsorbs alkali metal ions, so that the damage degree of the geopolymer structure is reduced, and the pore structure of the geopolymer is improved; the swelling molecules generated by the reaction of magnesium oxide and water also effectively compensate the self-shrinkage and drying shrinkage of magnesium oxide. Such multicomponent prepared geopolymer cements can have very beneficial corrosion resistance properties when zeolite and magnesia are incorporated as appropriate from the corrosion resistance coefficient point of view. This is because the structural stability of aluminosilicate gel reduces the rate of continuous diffusion of hydrogen ions, and because of the alkaline influence of the alkali-active activator, the hydration product is always more stable and not easily decomposed.
Claims (5)
1. A method for preparing a zeolitic geopolymer cement, comprising the steps of:
preparing a silicon-aluminum mixture: a. washing, filtering and drying large blocks of pure fine kaolin, then putting the large blocks of pure fine kaolin into a stainless steel tank of a planetary ball mill for grinding for 3 hours, screening the large blocks of pure fine kaolin, putting the large blocks of pure fine kaolin into a high-temperature furnace, and calcining the large blocks of pure fine kaolin for 2 hours at 700 ℃ to obtain metakaolin powder; b. mixing a certain amount of fly ash, zeolite, magnesium oxide and red mud, uniformly mixing and drying to obtain a silicon-aluminum mixture;
preparing an alkaline activator: : firstly, sodium hydroxide and a certain amount of water are melted to obtain a sodium hydroxide solution, then water glass is added to prepare alkali activity activators with different moduli, and the alkali activity activators are placed at normal temperature and cooled for 12 hours;
preparation of zeolitic geopolymer cement: slowly adding the silicon-aluminum mixture into an alkaline activator, adding distilled water while stirring until the liquid-solid ratio is 2/1, fully stirring, placing into an oven at 85 ℃, preserving for 12 hours, and demolding to obtain the zeolite geopolymer cementing material.
2. A process for the preparation of a zeolitic geopolymer cement according to claim 1, which comprisesCharacterized in that the step 1) specifically comprises the following steps: 100 parts of metakaolin, 10-15% of fly ash, 5-12% of zeolite, 1-5% of magnesium oxide and 10-15% of red mud, wherein the mass of the fly ash, the mass of the magnesium oxide and the mass of the red mud are respectively calculated according to the mass ratio of the metakaolin; the activity index of the metakaolin is more than or equal to 110; the fly ash is secondary fly ash, and the content of silicon dioxide is more than 45%; the zeolite is powder after grinding and screening, and the density is 2.27g/cm3The particle size is 100-120 meshes; the magnesium oxide is white amorphous powder, and the particle size of the magnesium oxide is less than 2 mu m; grinding the red mud by a ball mill for 40min, grinding and screening, wherein the fineness is more than 31 percent, and the ignition loss is less than 7 percent; the materials are prepared into a silicon-aluminum mixture according to the proportion, and the silicon-aluminum mixture is taken as 100 parts.
3. The method as claimed in claim 1, wherein the alkaline activator in step 2) is prepared from 190 parts of sodium hydroxide and 25-30 parts of water glass, the modulus of the water glass is 1.4, and the ratio of sodium hydroxide to active ingredient is more than 97%.
4. The method for preparing a zeolite geopolymer binding material as claimed in claim 1, wherein the distilled water in step 3) is added to satisfy a water-cement ratio of 0.35, which is the mass percentage of the mixture of water and silica-alumina, and water containing water glass and water produced by sodium hydroxide is removed.
5. The method for preparing a zeolite geopolymer gelled material as claimed in claim 1, wherein the prepared zeolite geopolymer gelled material is wrapped on a member by a preservative film at 45 ℃ for curing for 9 days, and then natural curing is carried out.
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| CN113003968A (en) * | 2021-05-07 | 2021-06-22 | 中国矿业大学 | Geopolymer dry powder material and preparation method thereof |
| CN113620306A (en) * | 2021-08-24 | 2021-11-09 | 广西民族大学 | Flower-type zeolite molecular sieve, preparation method and application thereof |
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| CN114196242A (en) * | 2022-01-14 | 2022-03-18 | 石河子大学 | Anti-cracking geopolymer-based inorganic powder coating and preparation method and application thereof |
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