CN110963742A - Coagulation accelerating type water dispersible concrete hydration temperature rise inhibitor and preparation method thereof - Google Patents
Coagulation accelerating type water dispersible concrete hydration temperature rise inhibitor and preparation method thereof Download PDFInfo
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- CN110963742A CN110963742A CN201811145219.5A CN201811145219A CN110963742A CN 110963742 A CN110963742 A CN 110963742A CN 201811145219 A CN201811145219 A CN 201811145219A CN 110963742 A CN110963742 A CN 110963742A
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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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Abstract
The invention relates to a concrete anti-cracking temperature control additive in the field of building materials, in particular to a set accelerating type water dispersible concrete hydration temperature rise inhibitor and a preparation method and application thereof. It is mainly formed by that amylopectin is catalyzed and hydrolyzed by aluminium sulfate, neutralized and added with alcohol amine compounds. The concrete hydration temperature rise inhibitor disclosed by the invention can be stably dispersed in water, and has the effects of not influencing the setting time of cement concrete, greatly reducing the hydration heat release rate of the cement and delaying the temperature peak time of structural concrete when being applied to the cement concrete.
Description
Technical Field
The invention belongs to the technical field of concrete admixtures, and particularly relates to a set accelerating type water dispersible concrete hydration temperature rise inhibitor and a preparation method thereof.
Background
The cement concrete is the most used building material in the world at present, and is widely applied to industries such as municipal administration, bridges, railways, water conservancy and hydropower. The cement concrete has the advantages of low price, convenient pouring and forming, high compressive strength and good durability, but has the defects of low flexural strength and small deformation when being used as a brittle material. After cement concrete is poured, a large amount of heat is released along with the hydration of cement, so that the temperature of a concrete structure rises rapidly in a short period, and the phenomenon is particularly obvious in a large-volume structure and a high-temperature season. Due to thermal expansion and cold contraction, the concrete cracks along with the gradual reduction of the temperature of the concrete to the service environment, and the cracking caused by the temperature contraction is the most important reason of the concrete structure engineering cracking. In order to solve the problem, measures such as reducing the using amount of cement, using a large-dosage mineral admixture, burying a cooling water pipe and the like are generally adopted in engineering, and the measures can improve or even avoid the generation of temperature cracks to a certain extent.
In recent years, scholars at home and abroad propose and develop a concrete hydration temperature rise inhibitor which can adjust cement hydration history, reduce hydration heat release rate and prolong concrete heat release time, thereby reducing the temperature peak of cement concrete after pouring and achieving the purpose of reducing temperature cracking. JP3729340B2 and JP4905977B2 disclose a product technology mainly comprising dextrin, and control of hydration heat release of cement is realized by controlling the solubility of the dextrin in cold water, and the applicant finds in research that the dextrin with certain solubility really has the effect of inhibiting the hydration temperature rise of concrete, but has the problems of remarkable temperature sensitivity and prolonged setting time. CN104098288B, CN104628296B, CN105039461B, CN105060762B disclose methods for preparing hydration heat inhibiting materials by using enzyme or acid catalyzed hydrolysis. The methods disclosed by CN103739722B, CN104592403B, CN104609766A, CN104609769B, CN104609770B, CN104610503B, CN104628297B, CN104710131B and CN104710132A propose cross-linking, alkoxylating, grafting, coating and modifying and the like to dextrin, thereby realizing the improvement of performance. The disclosed technology is focused on hydrolysis of starch by acid or enzyme, and is partially optimized by combining with a chemical modification strategy, and in an enzymolysis method, a specific enzyme is needed and a later-period inactivation step exists; in the acidolysis method, a step of neutralizing acid at the later stage exists, and most methods for preparing starch have procedures similar to washing and separation, so that the production procedures and cost are increased, and the yield of the product is reduced. The dextrin is used as a raw material to carry out chemical method modification, and the dextrin and the modifier are organic products, so that the defects of high technical difficulty and relatively high price exist, and the popularization of the dextrin in the field of relatively sensitive building materials is limited to a certain extent.
Disclosure of Invention
The invention provides a coagulation accelerating type water dispersible concrete hydration temperature rise inhibitor aiming at the problems of slow coagulation, low yield, washing and separation, high cost and the like in the prior art. In the research of the applicant, the aluminum sulfate is a cheap material with good coagulation promoting effect, and the aqueous solution of the aluminum sulfate is acidic and has the function of catalyzing the hydrolysis of starch. Further research shows that the amorphous aluminum hydroxide formed by neutralizing the aluminum sulfate aqueous solution with alkali metal carbonate such as sodium carbonate and potassium carbonate also has the cement concrete coagulation accelerating effect at low temperature, and the heat release amount of the amorphous aluminum hydroxide is smaller than that of aluminum sulfate in the process of accelerating the coagulation. Based on the above, the invention provides a coagulation accelerating type water dispersible concrete hydration temperature rise inhibitor, which is composed of a hydrolysis product of amylopectin catalyzed by aluminum sulfate, aluminum hydroxide, alkali metal sulfate and an alcamines compound, and the concrete proportion of each component is as follows:
the starch hydrolysate accounts for 20-80% of the total mass;
the aluminum sulfate, the aluminum hydroxide and the alkali metal sulfate are in any proportion, and the sum of the three components accounts for 10-60% of the total mass;
the molar mass ratio of the aluminum hydroxide to the alkali metal sulfate is 2: 3;
the alcamines compound accounts for 5-30% of the total mass.
The coagulation accelerating type water dispersible concrete hydration temperature rise inhibitor can be directly dispersed in water, and can keep long-term stability without layering, flocculation and other abnormal phenomena, and the preparation method comprises the following steps: adding amylopectin into 5-30wt% aluminum sulfate water solution under stirring, heating to 40-100 deg.C, heating for 2-48 hr, cooling to below 40 deg.C, adding alkali carbonate, stirring for 0.5-4 hr, and adding alcamines; the molar mass ratio of the alkali metal carbonate to the aluminum sulfate is (0: 1) - (3: 1).
In addition, the coagulation accelerating type water dispersible concrete hydration temperature rise inhibitor can also be prepared into a powder product by drying the water dispersible liquid, and the preparation method comprises the following steps: adding amylopectin into 5-30wt% aluminum sulfate water solution under stirring, heating to 40-100 deg.C, heating for 1-48 hr, cooling to below 40 deg.C, adding alkali carbonate, stirring for 0.5-4 hr, adding alcamines, and drying; the molar mass ratio of the alkali metal carbonate to the aluminum sulfate is (0: 1) - (3: 1). The drying mode is normal pressure drying or negative pressure drying, preferably spray drying, and the air inlet temperature during spray drying is not more than 300 ℃.
The invention defines the amylopectin as natural starch and modified starch thereof, preferably waxy corn starch, waxy glutinous rice starch and the like, wherein the amylopectin accounts for more than 95 percent of the total amylose and amylopectin in the starch.
Most of carbonate can be neutralized with the aluminum sulfate aqueous solution to form amorphous aluminum hydroxide. In the field of cement concrete, lithium salt, sodium salt and potassium salt have certain hydration excitation function, and are beneficial to promoting the development of setting time and early strength; the alkali metal sulfate is any one or a combination of lithium sulfate, sodium sulfate and potassium sulfate, and the alkali metal carbonate is any one or a combination of lithium carbonate, sodium carbonate and potassium carbonate.
The research also finds that the alcamines compounds with the coagulation promoting effect have complementary coagulation promoting effects on the stability and the coagulation time of the system, and are particularly effective for solving the sensitivity of cement.
The coagulation-promoting type water dispersible concrete hydration temperature rise inhibitor has good inhibition effect on cement hydration and temperature rise, is suitable for cement paste, mortar or concrete such as ordinary portland cement, sulphoaluminate cement and the like, and is particularly suitable for expansive concrete, the addition amount of the water dispersible concrete hydration temperature rise inhibitor is 0.1-10% of the mass of a glue material in a cement-based material, wherein a starch hydrolysate accounts for 0.02-5% of the mass of the glue material.
Detailed Description
In order to better understand the invention, the following examples are given for further illustration of the invention, but the invention is not limited to the scope of the examples.
Example 1
While stirring, 5g of aluminum sulfate was added to 95g of water, and the mixture was stirred until the aluminum sulfate was dissolved, thereby forming a transparent solution. Adding 20g of waxy corn starch, heating to 40 ℃, continuing to stir for 48h, stopping heating, beginning to cool, adding 1g of sodium carbonate, stirring for 0.5h, and adding 1.5g of triethanolamine to obtain the coagulation accelerating type water dispersible concrete hydration temperature rise inhibitor 1.
Example 2
While stirring, 30g of aluminum sulfate was added to 70g of water, and the mixture was stirred until the aluminum sulfate was dissolved, thereby forming a transparent solution. Adding 50g of waxy rice starch, heating to 100 ℃, continuing to stir for 2h, stopping heating, starting to cool, adding 3g of lithium carbonate and 2g of potassium carbonate when the temperature is lower than 40 ℃, stirring for 4h, and adding 15g of diethanolamine and 10g of triisopropanolamine to obtain the coagulation-promoting type water dispersible concrete hydration temperature rise inhibitor 2.
Example 3
20g of aluminum sulfate was added to 80g of water with stirring, and the mixture was stirred until the aluminum sulfate was dissolved to form a transparent solution. Adding 40g of glutinous rice starch, heating to 80 ℃, continuing stirring for 10h, stopping heating, starting cooling, adding 5g of lithium carbonate, sodium carbonate and potassium carbonate when the temperature is lower than 40 ℃, stirring for 2h, and adding 4g of diethanolamine, triethanolamine and triisopropanolamine respectively to obtain the coagulation promoting type water dispersible concrete hydration temperature rise inhibitor 3.
Example 4
20g of aluminum sulfate was added to 80g of water with stirring, and the mixture was stirred until the aluminum sulfate was dissolved to form a transparent solution. Adding 40g of glutinous rice starch, heating to 80 ℃, continuing stirring for 10h, stopping heating, starting cooling, and adding 4g of diethanolamine, triethanolamine and triisopropanolamine respectively when the temperature is lower than 40 ℃ to obtain the coagulation accelerating type water dispersible concrete hydration temperature rise inhibitor 4. And (3) carrying out spray drying on the obtained water dispersible concrete hydration temperature rise inhibitor 4 at the inlet air temperature of 250 ℃ to obtain powder, namely the coagulation accelerating concrete hydration temperature rise inhibitor 5.
Example 5
With stirring, 10g of aluminum sulfate was added to 90g of water, and the mixture was stirred until the aluminum sulfate was dissolved, thereby forming a transparent solution. Adding 25g of waxy corn starch and 25g of sticky rice starch respectively, heating to 80 ℃, continuing to stir for 10h, stopping heating, starting to cool, adding 1g of lithium carbonate, sodium carbonate and potassium carbonate respectively when the temperature is lower than 40 ℃, stirring for 2h, and adding 4g of diethanolamine, triethanolamine and triisopropanolamine respectively to obtain the coagulation promoting type water dispersible concrete hydration temperature rise inhibitor 6. And drying the obtained water dispersible concrete hydration temperature rise inhibitor 6 in a drying oven at normal temperature of 50 ℃ to obtain a powdery concrete hydration temperature rise inhibitor 7.
Comparative example 1
90g of an aqueous solution having a pH value adjusted by nitric acid and the same as that of the aluminum sulfate solution of example 5 was added with 25g each of waxy corn starch and glutinous rice starch, the temperature was raised to 80 ℃ and stirred for 10 hours, then the heating was stopped, the temperature was lowered, and after the pH value of the neutralization system was neutral, 1g each of lithium carbonate, sodium carbonate and potassium carbonate was added, and after stirring for 2 hours, 4g each of diethanolamine, triethanolamine and triisopropanolamine was added to obtain comparative example 1.
Comparative example 2
90g of an aqueous solution having a pH value adjusted by nitric acid and the same as that of the aluminum sulfate solution of example 5 was added with 25g of each of waxy corn starch and glutinous rice starch, the temperature was raised to 80 ℃ and stirred for 10 hours, then the heating was stopped and the temperature was lowered, and after the pH value of the neutralization system was neutral, 10g of aluminum sulfate was added, 1g of each of lithium carbonate, sodium carbonate and potassium carbonate was added after the aluminum sulfate solids disappeared, and 4g of each of diethanolamine, triethanolamine and triisopropanolamine was added after stirring for 2 hours, to obtain comparative example 2.
The performance evaluation is carried out by using the samples of the above-mentioned part of examples in cement concrete (or neat paste or mortar), and in the stability test, the powder sample No. 5 in example 4 and the powder sample No. 7 in example 5 are added with water to prepare 40% aqueous dispersion, and alternatively dextrin with cold water solubility of 50% is taken as a comparative example 3, and dextrin of comparative example 3 in the stability test is prepared into 40% aqueous dispersion.
In the sample evaluation, the stability of the sample is tested according to 7.11 items of JC/T1017-2006 Polymer emulsion for architectural waterproof coatings: filling about 0.5L of sample into a proper speed or glass container, leaving 10% of space in the bottle, sealing, placing into a constant temperature drying oven at (50 +/-2) DEG C, taking out after 14 days, placing at (23 +/-2) DEG C for 3h, opening the container, observing whether layering, flocculation and other phenomena exist, uniformly coating the sample on a glass plate by using a certain apparatus, and observing whether flocculate exists.
The cement adopted in the setting time and hydration heat tests is P.I type portland cement with 42.5 strength grade meeting the requirement of GB8076 annex A index. The setting time of the neat paste is tested according to the GB/T1346 method, the water-gel ratio is 0.35, the setting time difference is the difference value of the setting time of the neat paste added with the accelerating type water dispersible concrete hydration temperature rise inhibitor and the setting time of a standard non-doped sample, the unit is min, wherein, the positive value represents the delayed setting time, the negative value represents the shortened setting time, and the doping amount is the weight percentage of the starch hydrolysate in the glue material. The cement hydration heat release rate is measured by using a TAM AIR isothermal calorimeter of the company TA of America, the test temperature is 20 ℃, a test piece is pure slurry, the water-gel ratio is 0.4, the mixing amount is the weight percentage of a starch hydrolysate in cement, and the larger the peak value reduction amplitude of the cement hydration heat release rate under the same condition is, the better the performance of the cement hydration regulation material is.
As can be seen from the table, the coagulation accelerating type water dispersible concrete hydration temperature rise inhibitor has good water dispersion stability, compared with a comparative example, the coagulation accelerating type water dispersible concrete hydration temperature rise inhibitor has no abnormal conditions such as layering and flocculation, the layering phenomena occur in the comparative examples 1 and 3, and the layering and flocculation phenomena occur in the comparative example 2 with aluminum sulfate added later. The concrete hydration temperature rise inhibitor of the invention basically does not affect the setting time of cement paste, and even under high mixing amount, the concrete hydration temperature rise inhibitor also has the coagulation accelerating effect of shortening the setting time. In contrast, comparative example extended the setting time significantly, comparative example 1 without aluminum sulfate extended the setting time far beyond comparative example 2 with aluminum sulfate added; comparative example 3 dextrin extended the setting time even more than 7 days at high loadings.
The cement hydration heat release rate of the cement paste is measured by selecting the cement paste of the example 1 and the comparative example 3, wherein the mixing amount of the starch hydrolysate or the dextrin is 1.0 percent. In contrast to the baseline, both example 1 and comparative example 3 had the effect of reducing the maximum heat release rate, whereas the net slurry heat release of blend example 1 was substantially consistent with the baseline, both with an increase in heat release rate occurring shortly after addition of water, and the net slurry of blend comparative example 3 had an induction period of more than 50 hours before the heat release rate increased, meaning that it had a significant effect on the setting time, and this result was substantially consistent with the above-described setting time results.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. A coagulation-promoting type water dispersible concrete hydration temperature rise inhibitor is characterized in that: the catalyst consists of a hydrolysis product of amylopectin catalyzed by aluminum sulfate, aluminum hydroxide, alkali metal sulfate and an alcohol amine compound, wherein the specific proportion of each component is as follows:
the starch hydrolysate accounts for 20-80% of the total mass;
the aluminum sulfate, the aluminum hydroxide and the alkali metal sulfate are in any proportion, and the sum of the three components accounts for 10-60% of the total mass;
the molar mass ratio of the aluminum hydroxide to the alkali metal sulfate is 2: 3;
the alcamines compound accounts for 5-30% of the total mass.
2. The set-accelerating water dispersible concrete hydration temperature rise inhibitor according to claim 1, wherein: the amylopectin is natural starch and modified starch thereof, wherein the amylopectin accounts for more than 95% of the total amount of amylose and amylopectin, and waxy corn starch, waxy glutinous rice starch and the like are preferred; the alkali metal sulfate is any one or a combination of lithium sulfate, sodium sulfate and potassium sulfate; the alkali metal carbonate is any one or the combination of lithium carbonate, sodium carbonate or potassium carbonate; the alcamines compound is any one of or a combination of diethanolamine, triethanolamine or triisopropanolamine.
3. The method for preparing the accelerating hydration temperature rise inhibitor of the water dispersible concrete according to claim 1, wherein the accelerating hydration temperature rise inhibitor is prepared by adding amylopectin into 5-30wt% aluminum sulfate aqueous solution under stirring, heating to 40-100 ℃, heating for 2-48h, cooling to below 40 ℃, adding alkali carbonate, stirring for 0.5-4h, and adding an alcohol amine compound; wherein the molar mass ratio of the alkali metal carbonate to the aluminum sulfate is 0:1 to 3: 1.
4. The process for preparing the set-accelerating type water dispersible concrete hydration temperature rise inhibitor according to claim 1, wherein amylopectin is added into 5-30wt% aluminum sulfate aqueous solution under stirring, the temperature is raised to 40-100 ℃, the temperature is reduced to less than 40 ℃ after heating for 1-48h, alkali metal carbonate is added into the solution, the mixture is stirred for 0.5-4h, and then alcohol amine compound is added into the mixture and dried; the molar mass ratio of the alkali metal carbonate to the aluminum sulfate is 0:1 to 3: 1.
5. The method for preparing the set accelerating type water dispersible concrete hydration temperature rise inhibitor according to claim 3 or 4, characterized in that the amylopectin is natural starch and modified starch thereof, preferably waxy corn starch, waxy glutinous rice starch and the like, wherein the amylopectin accounts for more than 95% of the total amount of amylose and amylopectin in the starch; the alkali metal sulfate is any one or a combination of lithium sulfate, sodium sulfate and potassium sulfate; the alkali metal carbonate is any one or the combination of lithium carbonate, sodium carbonate or potassium carbonate; the alcamines compound is any one of or a combination of diethanolamine, triethanolamine or triisopropanolamine.
6. The method for preparing the accelerating water dispersible concrete hydration temperature rise inhibitor according to claim 5, wherein the drying manner is normal pressure drying or negative pressure drying.
7. The method for preparing the accelerating water dispersible concrete hydration temperature rise inhibitor according to claim 5, wherein the drying mode is spray drying, and the inlet air temperature during spray drying is not more than 300 ℃.
8. The use method of the accelerating setting type water dispersible concrete hydration temperature rise inhibitor according to claim 1 or 2, characterized in that the accelerating setting type water dispersible concrete hydration temperature rise inhibitor is mixed into cement paste, mortar or concrete, especially suitable for expansive concrete, the mixing amount of the accelerating setting type water dispersible concrete hydration temperature rise inhibitor is 0.1-10% of the mass of a cementing material, wherein a starch hydrolysate accounts for 0.02-5% of the mass of the cementing material.
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Cited By (2)
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| CN113831054A (en) * | 2021-08-26 | 2021-12-24 | 武汉三源特种建材有限责任公司 | Organic-inorganic composite cement hydration rate regulating material and preparation method thereof |
| CN114368929A (en) * | 2021-12-17 | 2022-04-19 | 武汉三源特种建材有限责任公司 | Cement hydration temperature rise inhibitor and preparation method and application thereof |
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| CN109311286B (en) * | 2016-05-31 | 2021-06-25 | 花王株式会社 | Absorbent article |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113831054A (en) * | 2021-08-26 | 2021-12-24 | 武汉三源特种建材有限责任公司 | Organic-inorganic composite cement hydration rate regulating material and preparation method thereof |
| CN114368929A (en) * | 2021-12-17 | 2022-04-19 | 武汉三源特种建材有限责任公司 | Cement hydration temperature rise inhibitor and preparation method and application thereof |
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