CN115611551B - Alkali aggregate composite inhibitor and preparation method thereof - Google Patents
Alkali aggregate composite inhibitor and preparation method thereof Download PDFInfo
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- CN115611551B CN115611551B CN202211621255.0A CN202211621255A CN115611551B CN 115611551 B CN115611551 B CN 115611551B CN 202211621255 A CN202211621255 A CN 202211621255A CN 115611551 B CN115611551 B CN 115611551B
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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
- C04B40/0042—Powdery mixtures
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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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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Abstract
The invention provides an alkali aggregate composite inhibitor and a preparation method thereof, wherein the preparation raw materials of the alkali aggregate composite inhibitor comprise the following components in parts by weight: 0.5-2.0 parts of titanate coupling agent, 15-30 parts of esterified product of polyethylene glycol and organic acid and 200-260 parts of mesoporous zeolite. The alkali aggregate composite inhibitor is beneficial to inhibiting the alkali aggregate reaction in the later stage of concrete, reducing the cracking risk in the later stage of concrete, improving the durability of concrete engineering and buildings and reducing the later maintenance cost of engineering projects.
Description
Technical Field
The invention relates to the field of concrete building materials, in particular to an alkali aggregate composite inhibitor and a preparation method thereof.
Background
In recent years, concrete materials have become the first building material worldwide due to their excellent cost performance. The concrete material is a composite material obtained by mixing and hardening a gelled material, coarse aggregate, fine aggregate and water. The main variety of the cementing material is cement, and the cement is subjected to hydration reaction after meeting water to bond coarse and fine aggregates together. Since the international energy crisis in the last 70 th century, the cement industry gradually changes wet method into dry method production, so that the alkali content of cement is increased. Particularly, in the later period of 80 years, as a measure for utilizing industrial waste and saving energy, the recycled high-alkali kiln ash is doped into cement as an advanced measure to be popularized nationwide, so that the alkali content of domestic cement is greatly increased, the PH of pore liquid is greater than 12 in the hydration process, and the pore liquid is highly alkaline. In addition, both coarse and fine aggregates, although natural and man-made, are derived from rock material. The kinds of rocks are various, such as pyrophyllite, serpentine, illite, chlorite, mica, talc, kaolinite, vermiculite, igneous rock, metamorphic rock, sedimentary rock and the like. The latter three kinds of rock ore contain strain quartz, active silicon dioxide and microcrystalline quartz. In humid and watery conditions, slow chemical reactions of these reactive components also occur in the hardened concrete.
The alkali-aggregate reaction is that alkali in cement and active silica in aggregate slowly react to generate silicate gel, the silicate gel has larger and larger output after long-term accumulation and strong water absorption, and the volume of the silicate gel expands, so that the expansion stress of a concrete structure from inside to outside is caused, the concrete cracks, the mechanical property of the concrete is reduced, and the durability of the concrete is damaged. Alkali aggregate reaction cracking is found in some airport concrete runways in China, and after some urban highway traffic is built for several years, cracking and sampling of wet parts of the urban highway traffic prove that the alkali aggregate reaction is realized.
Those skilled in the art currently try to control the development of alkali-aggregate reactions in a manner that blocks the source of moisture, but this solution works poorly because the water vapor is non-porous. Although the alkali content of cement is controlled to inhibit the alkali-aggregate reaction of concrete, the alkali content of cement is not limited in GB175-2007 "general portland cement", so inhibiting the alkali content of cement to inhibit the alkali-aggregate reaction of concrete requires custom production of cement materials, and the implementation difficulty is large for many engineering projects in view of cost and production efficiency. The aggregate is limited, active coarse and fine aggregates are not used, and under the form that the supply and demand of the sand and stone materials are increasingly tense, a plurality of projects can not be applied to the active aggregate inevitably, and building waste can be used as a raw material in the future. The common method is to replace part of cementing materials, such as silica fume, fly ash and the like, with admixture by 20-30% of cement amount, so as to reduce the alkali content in the cement, and from the application result, the admixture has certain effect of inhibiting the concrete alkali aggregate reaction, but the disadvantage is that the admixture is large in amount and the effect is still to be improved.
Disclosure of Invention
In view of the above, the present invention provides an alkali-aggregate composite inhibitor for inhibiting concrete alkali-aggregate reaction.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
the alkali aggregate composite inhibitor comprises the following raw materials in parts by weight: titanate coupling agent 0.5-2.0 weight portions, esterified matter of polyglycol and organic acid 15-30 weight portions, and mesoporous zeolite 200-260 weight portions.
The alkali aggregate composite inhibitor can be used in concrete containing amorphous or poorly crystalline silicon dioxide in sandstone aggregate, is favorable for inhibiting alkali aggregate reaction in the later period of the concrete, reduces the cracking risk in the later period of the concrete, improves the durability of concrete engineering and buildings, and reduces the later maintenance cost of engineering projects. The invention can be used in normal concrete, pump concrete and precast concrete, and can be widely used in industrial and civil engineering.
Further, the titanate coupling agent comprises at least one of di (triethanolamine) diisopropyl titanate, a chelate of bis (dioctyloxypyrophosphate) ethylene titanate and triethanolamine, isopropyltris (dioctylphosphonoxy) titanate, isopropyldioleate acyloxy (dioctylphosphonoxy) titanate.
Further, the molar ratio of the alkyd in the esterified product of the polyethylene glycol and the organic acid is (5-8): (12-18).
Further, the polyethylene glycol has a weight average molecular weight of 200 to 600.
Further, the organic acid is at least one of formic acid, acetic acid and propionic acid.
Further, the medium pore zeolite includes at least one of ferrierite, Y zeolite and ZSM-5 zeolite.
The invention also provides a preparation method of the alkali aggregate composite inhibitor, which comprises the following steps:
adding mesoporous zeolite into a kneader, heating to 60-65 ℃, adding an esterified product of polyethylene glycol and organic acid, kneading for 1.0-1.5 hours, then adding a titanate coupling agent, kneading for 1.5-2 hours, and cooling to room temperature to obtain the alkali aggregate composite inhibitor.
Further, the preparation method of the esterified product of the polyethylene glycol and the organic acid comprises the following steps:
mixing polyethylene glycol, organic acid, catalyst and dehydrating agent uniformly, heating to 60-65 deg.C, and keeping the temperature.
Further, the catalyst is phosphotungstic heteropoly acid and SO 4 2- /SiO 2 -TiO 2 At least one of cerium sulfate and zirconium sulfate.
Further, the dehydrating agent is at least one of calcium oxide and anhydrous calcium sulfate.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The experimental procedures in the following examples are all conventional ones unless otherwise specified. The test materials used in the following examples were purchased from a conventional biochemical reagent store unless otherwise specified. In addition, unless otherwise specified, all terms and processes related to the present embodiment should be understood according to the conventional knowledge and conventional methods in the art.
The alkali aggregate composite inhibitor comprises the following raw materials in parts by weight: titanate coupling agent 0.5-2.0 weight portions, esterified matter of polyglycol and organic acid 15-30 weight portions, and mesoporous zeolite 200-260 weight portions.
The alkali aggregate composite inhibitor of the invention is composed of three main components, namely a titanate coupling agent, an esterified product of polyethylene glycol and organic acid and mesoporous zeolite powder. The mesoporous zeolite powder can adsorb the titanate coupling agent and the esterified product of polyethylene glycol and organic acid by means of its own porous structure, so that the adsorbed titanate coupling agent and the esterified product of polyethylene glycol and organic acid can be slowly released in the hardened concrete system to exert long-acting effect. In addition, the mesoporous zeolite can adsorb K + ions and Na + in hardened concrete, so that the concentration of soluble alkaline ions is reduced, and further, the ionization of hydroxyl in a system is inhibited, the pH value of the system is reduced, and the effect of inhibiting the alkali aggregate reaction is achieved. The medium pore size zeolite can be selected from at least one of ferrierite, Y zeolite and ZSM-5 zeolite.
The titanate coupling agent component can perform hydrophobic modification on active silica on the surface of aggregate, and can reduce the wetting effect of water molecules on active silicon dioxide in hardened concrete in a humid environment, thereby being beneficial to inhibiting the reaction of alkaline ions and the active silica in the hardened concrete. The long carbon chain hydrophobic group of the titanate coupling agent is grafted to the surface of the aggregate, and can perform hydrophobic modification on active silicon dioxide on the surface of the aggregate, so that the silicon dioxide on the surface of the aggregate has a hydrophobic effect, water cannot be attached to the surface of the aggregate, the wetting effect of water molecules on active silicon dioxide in hardened concrete in a humid environment is reduced, hydroxide ions cannot be ionized by alkaline substances, and the alkaline ions in the hardened concrete can be favorably inhibited from reacting with the active silicon dioxide. In addition, the titanium element contained in the titanate coupling agent can improve the durability of the concrete, and a proper amount of titanium dioxide is beneficial to improving the self-cleaning performance of the concrete. The titanate coupling agent may preferably employ at least one member selected from the group consisting of diisopropyl di (triethanolamine) titanate, a chelate of ethylene bis (dioctyloxypyrophosphate) titanate and triethanolamine, isopropyltris (dioctylphosphonoxy) titanate, isopropyldioleacyloxy (dioctylphosphonoxy) titanate.
The esterification product of polyethylene glycol and organic acid is hydrolyzed under alkaline condition to generate organic acid, neutralize alkali in the system, reduce pH value of hardened concrete and inhibit alkali aggregate reaction. The molar ratio of the preferred polyethylene glycol to the alkyd in the ester of the organic acid is (5-8): (12-18). The polyethylene glycol has a weight average molecular weight of 200-600. The molecular weight in the range is small, the esterification efficiency is high, and more organic acid can be released by hydrolysis. The organic acid may preferably be at least one of formic acid, acetic acid and propionic acid. The organic acid has strong acidity and higher alkali neutralization efficiency.
The invention also provides a preparation method of the alkali aggregate composite inhibitor, which comprises the following steps:
preparation of esterified product of polyethylene glycol with organic acid:
adding 0.5-0.8mol of polyethylene glycol into a reactor, starting an oil bath heater, setting the temperature to be 60-65 ℃, starting stirring, adding 1.2-1.8mol of organic acid monomers and a catalyst, reacting for 2-3 hours, adding a dehydrating agent, continuing to react for 2-3 hours, continuing to add the dehydrating agent, and cooling to room temperature to obtain a viscous pasty esterified product of polyethylene glycol and organic acid. The catalyst used in this step is 0.1-0.3% of the mass of the reactants, and it may preferably be phosphotungstic heteropoly acid, SO 4 2- /SiO 2 -TiO 2 At least one of cerium sulfate and zirconium sulfate has high catalytic efficiency compared with common concentrated sulfuric acid. The total amount of the dehydrating agent used is 0.5 to 1.0mol, and at least one of calcium oxide and anhydrous calcium sulfate may be preferable. The catalyst and dehydrating agent may be removed without additional removal.
Preparing an alkali aggregate composite inhibitor:
adding mesoporous zeolite powder into a kneading machine, heating to 60-65 ℃, adding an esterified product of polyethylene glycol and organic acid, kneading for 1.0-1.5 hours, then adding a titanate coupling agent, kneading for 1.5-2 hours, and cooling to room temperature to obtain the alkali aggregate composite inhibitor. The above-mentioned reagents are commercially available.
The following describes in detail specific embodiments of the present invention.
Example 1
The preparation method of the esterified product of the polyethylene glycol and the organic acid comprises the following process steps: firstly, 0.8mol of polyethylene glycol with the weight-average molecular weight of 200 is added into a reactor, an oil bath heater is started, the temperature is set to be 62 ℃, stirring is started, 1.8mol of formic acid and 0.36 g of zirconium sulfate are added, after the reaction is carried out for 3 hours, 28 g of calcium oxide is added, the reaction is continued for 3 hours, 28 g of calcium oxide is added, and the thick paste is cooled to the room temperature, so that the esterified substance of the polyethylene glycol and the organic acid is obtained.
Preparing an alkali aggregate composite inhibitor: adding 210g of mesoporous Y-type zeolite powder into a kneader, heating to 62 ℃, adding 16g of esterified product of polyethylene glycol and organic acid, kneading for 1.2 hours, adding 1.0g of isopropyl tri (dioctyl phosphate acyloxy) titanate, kneading for 1.5 hours, and cooling to room temperature to obtain the powdery alkali aggregate composite inhibitor.
Example 2
The preparation method of the esterified product of the polyethylene glycol and the organic acid comprises the following process steps: firstly, 0.6mol of polyethylene glycol with the weight-average molecular weight of 400 is added into a reactor, an oil bath heater is started, the set temperature is 65 ℃, stirring is started, 1.4mol of acetic acid and 0.32 g of phosphotungstic heteropoly acid are added, after the reaction is carried out for 2 hours, 35 g of calcium sulfate is added, the reaction is carried out for 3 hours, 35 g of calcium sulfate is continuously added, and the mixture is cooled to the room temperature to obtain a viscous paste, so that the esterified product of the polyethylene glycol and the organic acid is obtained.
Preparing an alkali aggregate composite inhibitor: adding 260g of mesoporous ferrierite powder into a kneader, heating to 62 ℃, adding 30g of esterified substance of polyethylene glycol and organic acid, kneading for 1.5 hours, adding 2.0g of chelate of bis (dioctyloxy pyrophosphate) ethylene titanate and triethanolamine, kneading for 2 hours, and cooling to room temperature to obtain the powdery alkali aggregate composite inhibitor.
Example 3
The preparation method of the esterification product of polyethylene glycol and organic acid comprises the following processThe method comprises the following steps: firstly, 0.5mol of polyethylene glycol with the weight-average molecular weight of 600 is added into a reactor, an oil bath heater is started, the set temperature is 65 ℃, stirring is started, 0.6mol of formic acid is added 4 2- /SiO 2 -TiO 2 0.2 g of catalyst, after 2.5 hours of reaction, 30g of calcium oxide was added, and 0.6mol of acetic acid and 0.18 g of SO were further added 4 2- /SiO 2 -TiO 2 And (3) reacting for 2.5 hours by using a catalyst, adding 30g of calcium oxide, and cooling to room temperature to obtain a viscous paste, namely an esterified product of polyethylene glycol and organic acid.
The preparation method of the alkali aggregate composite inhibitor comprises the following steps: 230g of ZSM-5 mesoporous zeolite powder is added into a kneader, the mixture is heated to 60 ℃, 25g of esterified product of polyethylene glycol and organic acid is added, the mixture is kneaded for 1.5 hours, 2g of chelate of bis (dioctyloxypyrophosphate) ethylene titanate and triethanolamine is added, the mixture is kneaded for 1.5 hours, and the mixture is cooled to room temperature to obtain the powdery alkali aggregate composite inhibitor.
Example 4
The preparation method of the ester of the polyethylene glycol and the organic acid comprises the following process steps: firstly, 0.4mol of polyethylene glycol with the weight-average molecular weight of 200 and 400 respectively is added into a reactor, an oil bath heater is started, the temperature is set to be 63 ℃, stirring is started, 1.8mol of propionic acid is added 4 2- /SiO 2 -TiO 2 0.3 g of catalyst, reacting for 3 hours, adding 36 g of calcium sulfate, and continuously adding SO 4 2- /SiO 2 -TiO 2 0.2 g of catalyst is added for reaction for 3 hours, 36 g of calcium sulfate is added, and the mixture is cooled to room temperature to obtain viscous paste, namely the esterified product of polyethylene glycol and organic acid.
Preparing an alkali aggregate composite inhibitor: adding 260g of ZSM-5 zeolite mesoporous zeolite powder into a kneader, heating to 65 ℃, adding 20g of esterified product of polyethylene glycol and organic acid, kneading for 1.5 hours, adding 1g of each of chelate of bis (dioctyloxypyrophosphate) ethylene titanate and triethanolamine and isopropyl tris (dioctylphosphonoyl) titanate, kneading for 1.8 hours, and cooling to room temperature to obtain a powdery mixture.
The above examples 1-4 were used for alkali aggregate reaction tests. Prior to testing, the machine-made sand in the stockpile was lithographically analyzed as granite and contained the reactive mineral strained quartz at about 38%. The samples of examples 1-4 were subjected to alkali-aggregate reaction testing according to GB/T14684-2011, the cement was a general portland cement of Cheng Dynasty PO.42.5, and the coal ash used was first grade ash. The sand is classified firstly, and is screened by a square hole screen, so that the sand with the grain diameter of more than 4.75mm and less than 0.15mm is screened out. The mass of each fraction of the sand for alkali-aggregate reaction experiment is shown in table 1:
TABLE 1 quality of each grade of sand for alkali-aggregate reaction
440 g of cementing material, 990 g of sand and a certain amount of water are weighed for a mortar experiment, and the water consumption for the experiment is determined according to GB 2419. The jumping frequency of the jumping table is 6s and 10 times of jumping, and the fluidity is based on 105 mm-120 mm. The mortar stirring is carried out according to the GB/T17671, after the stirring is finished, the mortar is immediately filled into a test mould which is provided with an expansion measuring head for 40 times in each layer, the periphery of the expansion measuring head is carefully tamped, after the pouring, the excessive mortar is scraped by a steamed bread knife, and the mortar is trowelled, numbered and shows the length measuring direction, and 3 groups of test forming are carried out in each group. And then maintaining according to GB/T14684-2011, testing and calculating the expansion rate of the test block for 14 days, 30 days, 60 days and 180 days, and observing and recording the appearance condition of the test block at each age. The test results are shown in table 2:
table 2 alkali aggregate reaction test results
As can be seen from Table 2, in experiment 1, the test block appeared crisp in 180 days, the expansion rate of the test block reached 0.5%, the expansion rate of the test block in 14 days was 0.12%, and the requirement that the expansion rate of the test block in 180 days in GB14684-2011 is far less than 0.1%, which indicates that the alkali-aggregate reaction is serious. In experiment 2, the grade 1 fly ash is used for replacing 30% of cement, the expansion rate of the test block is less than 0.1% in the first 30 days, but the expansion rate of the test block reaches 0.1% in 60 days, and the expansion rate of the test block reaches 0.18% in 180 days, which shows that the fly ash reduces the alkali-aggregate reaction to a certain extent, but can not meet the standard requirement. After the samples 1-4 are adopted, the mixing amount is 3 percent of the glue material, the test block with 180 days has no obvious cracks, the expansion rate is less than 0.1 percent, and the alkali aggregate reaction is completely inhibited. In conclusion, the alkali aggregate composite inhibitor provided by the invention has the advantages of low mixing amount and good inhibition effect, and has an energy-saving and synergistic effect on building engineering.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
Claims (8)
1. An alkali aggregate composite inhibitor is characterized in that: the preparation raw materials of the alkali aggregate composite inhibitor comprise the following components in parts by weight: titanate coupling agent 0.5-2.0 weight portions, esterified matter of polyglycol and organic acid 15-30 weight portions, and mesoporous zeolite 200-260 weight portions; the intermediate pore size zeolite comprises at least one of ferrierite, a Y zeolite and a ZSM-5 zeolite;
the preparation method of the esterified product of the polyethylene glycol and the organic acid comprises the following steps:
mixing polyethylene glycol, organic acid, catalyst and dehydrating agent uniformly, heating to 60-65 deg.C, and keeping the temperature.
2. The alkali-aggregate composite inhibitor according to claim 1, characterized in that: the titanate coupling agent comprises at least one of di (triethanolamine) diisopropyl titanate, a chelate of bis (dioctyloxypyrophosphate) ethylene titanate and triethanolamine, isopropyltris (dioctylphosphonoxy) titanate and isopropyldioleate acyloxy (dioctylphosphonoxy) titanate.
3. The alkali-aggregate composite inhibitor according to claim 1, characterized in that: the molar ratio of the alkyd in the esterified product of the polyethylene glycol and the organic acid is (5-8): (12-18).
4. The alkali-aggregate composite inhibitor according to claim 1, characterized in that: the weight average molecular weight of the polyethylene glycol is 200-600.
5. The alkali-aggregate composite inhibitor according to claim 1, characterized in that: the organic acid is at least one of formic acid, acetic acid and propionic acid.
6. A preparation method of the alkali-aggregate composite inhibitor according to any one of claims 1 to 5, wherein the method comprises the following steps:
adding mesoporous zeolite into a kneader, heating to 60-65 ℃, adding an esterified product of polyethylene glycol and organic acid, kneading for 1.0-1.5 hours, then adding a titanate coupling agent, kneading for 1.5-2 hours, and cooling to room temperature to obtain the alkali aggregate composite inhibitor.
7. The method for preparing the alkali-aggregate composite inhibitor according to claim 6, wherein the method comprises the following steps: the catalyst is phosphotungstic heteropoly acid and SO 4 2- /SiO 2 -TiO 2 At least one of cerium sulfate and zirconium sulfate.
8. The method for preparing the alkali-aggregate composite inhibitor according to claim 6 or 7, wherein: the dehydrating agent is at least one of calcium oxide and anhydrous calcium sulfate.
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| CN202211621255.0A CN115611551B (en) | 2022-12-16 | 2022-12-16 | Alkali aggregate composite inhibitor and preparation method thereof |
| PCT/CN2023/083638 WO2024124734A1 (en) | 2022-12-16 | 2023-03-24 | Alkali aggregate composite inhibitor and preparation method therefor |
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| JP2022134233A (en) * | 2021-03-03 | 2022-09-15 | Ｕｂｅ三菱セメント株式会社 | Cement composition and production method thereof, alkali silica reaction inhibitor, inhibition method of alkali silica reaction |
| CN115611551B (en) * | 2022-12-16 | 2023-03-14 | 石家庄市长安育才建材有限公司 | Alkali aggregate composite inhibitor and preparation method thereof |
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| WO2024124734A1 (en) | 2024-06-20 |
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