CN110963733A - Preparation method of water-based cement hydration rate regulating material - Google Patents
Preparation method of water-based cement hydration rate regulating material Download PDFInfo
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- CN110963733A CN110963733A CN201811145005.8A CN201811145005A CN110963733A CN 110963733 A CN110963733 A CN 110963733A CN 201811145005 A CN201811145005 A CN 201811145005A CN 110963733 A CN110963733 A CN 110963733A
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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
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/16—Sulfur-containing compounds
- C04B24/161—Macromolecular compounds comprising sulfonate or sulfate groups
- C04B24/168—Polysaccharide derivatives, e.g. starch sulfate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention belongs to the field of concrete admixtures, and particularly relates to a cement hydration rate regulating material and a preparation method thereof, wherein the water-based cement hydration rate regulating material is prepared by grafting a hydrophilic polymer monomer onto a starch molecule; the preparation method is to polymerize the hydrophilic polymer monomer by a free radical polymerization method, the starch solution obtained by the method has a good cement hydration rate regulating effect, the influence of hydration regulation caused by uneven stirring of the solid cement hydration rate regulating material is effectively solved, the preparation process is simple, the drying of a solid finished product and the use of an organic solvent are reduced, and the preparation method accords with the theme of green chemistry.
Description
Technical Field
The invention belongs to the field of concrete admixtures, and particularly relates to a preparation method of an aqueous cement hydration rate regulating material.
Background
The crack control problem is a problem that large-volume concrete must be regarded during construction. Temperature cracking is one of the most common forms of cracking in large volumes of concrete. In the construction process of mass concrete, because cement is hydrated to emit a large amount of heat and the heat dissipation is not timely, the temperature difference between the inside and the outside of the concrete is increased rapidly, and great temperature stress is generated, so that cracks are generated, and finally serious consequences are caused.
In order to reduce the generation of temperature cracks, the method not only improves the heat dissipation efficiency, but also regulates and controls the hydration of the cement, reduces the hydration rate of the cement, and further reduces the temperature peak heat release, and is an effective method.
Such materials for regulating cement hydration have been extensively studied.
CN104610503A selects dextrin to carry out cross-linking reaction with a cross-linking agent in the presence of a redox initiator, so as to obtain a hydration regulation material which has a spatial structure, is acid-resistant, alkali-resistant and shear-resistant and can effectively reduce the peak value of the hydration heat release rate.
CN104710131A is coated with insoluble polymer to modify dextrin, so as to obtain a hydration heat regulating material which can effectively reduce hydration rates in an acceleration period and a deceleration period and has little influence on a cement hydration induction period.
CN104628296A is prepared by reacting starch with an acid catalyst and a cross-linking agent, and then reacting with alkenyl succinic anhydride, thereby preparing a regulating material which has a spatial network structure, high acid-base resistance and high shearing capacity and can effectively reduce hydration heat release rate.
CN105060762B discloses a preparation method of a starch-based hydration heat regulating material, which is characterized in that starch is completely gelatinized and then is added with enzyme for hydrolysis, ethanol is added for precipitation, filtration and pulverization to obtain dextrin, and the dextrin is continuously reacted with an emulsifier to prepare the starch-based hydration heat regulating material with hydration regulating effect.
The above patent documents are all materials with excellent cement hydration regulation and control functions, but the prepared products are all solid products, and are not uniformly stirred in the construction process, so that the hydration regulation and control functions are greatly influenced. Compared with the above patents, the method reduces the steps of using organic solvent and drying in the preparation process, and the preparation process is simpler. The invention designs the water aqua cement hydration rate regulating material which can be used together with the water reducing agent from the construction angle, and effectively solves the problem of uneven stirring of the solid hydration heat regulating material.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide an aqueous cement hydration rate regulating material and a preparation method thereof.
At present, most dextrin or starch-based cement hydration regulation and control materials are solid materials, and different stirring modes cause uneven distribution of hydration heat regulation and control materials, so that the hydration regulation and control effect is influenced to a great extent. The solubility of the starch base can be increased by properly modifying the starch base and introducing hydrophilic groups, so that the starch base is dispersed more uniformly and plays a better hydration regulation role.
The invention adopts the following specific technical scheme:
the preparation method of the water aqua cement hydration rate regulating material, which is a starch solution grafted with a water-soluble polymer, comprises the following steps:
mixing starch and water to prepare 10-20wt% of starch milk, adding inorganic acid for catalysis, adjusting the pH to 1, heating to 50-70 ℃, and preserving heat for 4-8 hours;
and (3) adjusting the pH value to 7, adding a water-soluble polymer monomer and an initiator, and carrying out heat preservation reaction for 8-12 h to obtain the water aqua hydration rate regulating material.
In a further improvement of the invention, the inorganic acid is one of hydrochloric acid, sulfuric acid or nitric acid, and the initiator is ammonium persulfate.
The invention further improves that the starch is one of wheat starch, soluble starch, cassava starch, glutinous starch, lotus root starch and pumpkin starch.
In a further improvement of the invention, the monomer of the water-soluble polymer is one or more of vinyl pyrrolidone, 2-acrylamide-2-methylpropanesulfonic acid, N-vinyl formamide and sodium vinylsulfonate.
In a further development of the invention, water-soluble polymers are grafted, the amount of monomers being 10 to 40%, preferably 15 to 25%, based on the mass of the starch.
Detailed Description
In order to enhance the understanding of the present invention, the present invention will be described in further detail with reference to the following examples, which are provided for the purpose of illustration only and are not intended to limit the scope of the present invention.
In the examples of the present invention, no particular description is given, and all the cements used are 52.5 cement for small open-field. 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 ℃, the test piece is pure slurry, the water-gel ratio is 0.4, and the addition percentage of the cement hydration regulation material is relative to the mass of the gel material. The maximum heat release rate peak value reduction amplitude is used as a judgment standard of the performance of the hydration regulation material, and the larger the heat release rate peak value reduction amplitude under the same condition is, the better the performance of the cement hydration regulation material is. The test method is described in GB/T2022-1980.
In the embodiment of the invention, the concrete mixing proportion adopted in the test is as follows: 320kg/m cement380kg/m of fly ash3753kg/m river sand31084 kg/m coarse aggregate3160 kg/m of water3The fly ash is first-grade fly ash, the sand is medium sand with fineness modulus of 2.6, and the stones are continuous graded broken stones with particle size of 5-20 mm.
The concrete adiabatic temperature rise is measured BY using a BY-ATC/JR adiabatic temperature rise instrument of Bo Yuan science and technology development Limited company in Zhoushan, and the initial temperature of the adiabatic temperature rise test is 15 ℃.
The concrete compressive strength and the setting time are executed according to GB/T50081-2002 Standard for testing the mechanical properties of common concrete.
Example 1
The preparation of the water aqua cement hydration rate regulating material comprises the following steps: adding 100g of pumpkin starch into water to prepare 10wt% of starch milk, adjusting the pH value to 1 by using hydrochloric acid, heating to 50 ℃, keeping the temperature for 8 hours, adjusting the pH value to 7 by using sodium carbonate, adding 20g of vinyl pyrrolidone, 20g of 2-acrylamide-2-methylpropanesulfonic acid and 1.8g of ammonium persulfate, and keeping the temperature for 8 hours to obtain the water-based cement hydration rate regulating material product.
Example 2
The preparation of the water aqua cement hydration rate regulating material comprises the following steps: adding 100g of waxy starch into water to prepare 20wt% starch milk, adjusting the pH value to 1 by hydrochloric acid, heating to 53 ℃, preserving heat for 4 hours, adjusting the pH value to 7 by sodium carbonate, adding 10g of 2-acrylamide-2-methylpropanesulfonic acid and 1.1g of ammonium persulfate, and continuously preserving heat for 8.5 hours to obtain the water-based cement hydration rate regulating material product.
Example 3
The preparation of the water aqua cement hydration rate regulating material comprises the following steps: adding 100g of wheat starch into water to prepare 15wt% of starch milk, adjusting the pH value to 1 by hydrochloric acid, heating to 56 ℃, preserving the heat for 5 hours, adjusting the pH value to 7 by sodium carbonate, adding 15g N-vinylformamide and 2.1g of ammonium persulfate, and continuously preserving the heat for 10 hours to obtain the water-based cement hydration rate regulating material product.
Example 4
The preparation of the water aqua cement hydration rate regulating material comprises the following steps: adding 100g of lotus root starch into water to prepare 13wt% of starch milk, regulating the pH value to 1 by using hydrochloric acid, heating to 70 ℃, preserving the heat for 7 hours, regulating the pH value to 7 by using sodium carbonate, adding 25g N-vinylformamide and 2.5g of ammonium persulfate, and continuously preserving the heat for 9.5 hours to obtain the water-based cement hydration rate regulating material product.
Example 5
The preparation of the water aqua cement hydration rate regulating material comprises the following steps: adding 100g of soluble starch into water to prepare 17wt% of starch milk, adjusting the pH value to 1 by hydrochloric acid, heating to 60 ℃, preserving heat for 7.5h, adjusting the pH value to 7 by sodium carbonate, adding 18g of sodium vinylsulfonate and 1.6g of ammonium persulfate, and continuously preserving heat for 8.7h to obtain the water-based cement hydration rate regulating material product.
Example 6
The preparation of the water aqua cement hydration rate regulating material comprises the following steps: adding 100g of cassava starch into water to prepare 14wt% of starch milk, adjusting the pH value to 1 by using sulfuric acid, heating to 65 ℃, keeping the temperature for 6h, adjusting the pH value to 7 by using sodium carbonate, adding 24g of sodium vinylsulfonate and 2.6g of ammonium persulfate, and keeping the temperature for 11h to obtain the water-based cement hydration rate regulating material product.
Example 7
The preparation of the water aqua cement hydration rate regulating material comprises the following steps: adding 100g of cassava starch into water to prepare 18wt% of starch milk, regulating the pH value to 1 by hydrochloric acid, heating to 66 ℃, preserving heat for 6.5 hours, regulating the pH value to 7 by sodium carbonate, adding 25g of vinyl pyrrolidone and 1.7g of ammonium persulfate, and continuously preserving heat for 9 hours to obtain the water-based cement hydration rate regulating material product.
Example 8
The preparation of the water aqua cement hydration rate regulating material comprises the following steps: adding 100g of pumpkin starch into water to prepare 19wt% of starch milk, adjusting the pH value to 1 by using nitric acid, heating to 68 ℃, preserving heat for 5.5 hours, adjusting the pH value to 7 by using sodium carbonate, adding 30g of 2-acrylamide-2-methylpropanesulfonic acid and 1.5g of ammonium persulfate, and continuously preserving heat for 12 hours to obtain the water-based cement hydration rate regulating material product.
Comparative example 1
Unmodified 15wt% starch emulsion
Comparative example 2
15wt% glucose solution
Comparative example 3
Hydration heat regulating material was prepared by referring to CN105712647A example 1.
TABLE 1
| Numbering | Mixing amount/% | Coagulation time/hour | 28 day compressive strength/MPa | Maximum rate of hydration decrease peak/%) |
| Example 1 | 0.2 | 9.7 | 51.1 | 83.1 |
| Example 2 | 0.2 | 11.5 | 50.7 | 83.6 |
| Example 3 | 0.2 | 10.6 | 49.1 | 82.4 |
| Example 4 | 0.5 | 9.3 | 48.9 | 86.1 |
| Example 5 | 0.8 | 12.1 | 48.7 | 88.4 |
| Example 6 | 0.8 | 11.9 | 48.1 | 89.1 |
| Example 7 | 0.6 | 9.3 | 48.9 | 88.1 |
| Example 8 | 0.6 | 10.8 | 49.3 | 87.3 |
| Comparative example 1 | 0.2 | 7.7 | 52.1 | 0 |
| Comparative example 2 | 0.2 | 12.3 | 45.2 | 1.3 |
| Comparative example 3 | 0.2 | 10.1 | 50.1 | 85.0 |
As can be seen from Table 1, the acid catalyst and the hydrophilic polymer monomer are sequentially introduced into the starch, so that the hydrophilicity of the starch is improved, the starch exists in a solution form, the preparation process is simple, the cost is low, and compared with a solid product, the drying link is reduced, and the production cost is reduced; the whole production process takes water as a medium, the process is green and environment-friendly, and the peak value of the hydration heat release rate can be effectively reduced under the condition that the obtained water aqua hydration heat regulation material hardly influences the strength and the setting time.
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 (6)
1. A preparation method of an aqueous cement hydration rate regulating material is characterized by comprising the following steps: the cement hydration rate regulating material is a starch solution grafted with a water-soluble polymer, and comprises the following steps:
mixing starch and water to prepare 10-20wt% of starch milk, adding inorganic acid for catalysis, adjusting the pH to 1, heating to 50-70 ℃, and preserving heat for 4-8 hours;
and (3) adjusting the pH value to 7, adding a water-soluble polymer monomer and an initiator, and carrying out heat preservation reaction for 8-12 h to obtain the water aqua hydration rate regulating material.
2. The preparation method of the aqueous cement hydration rate regulating material as claimed in claim 1, wherein: the inorganic acid is one of hydrochloric acid, sulfuric acid or nitric acid, and the initiator is ammonium persulfate.
3. The preparation method of the aqueous cement hydration rate regulating material as claimed in claim 1, wherein: the starch is one of wheat starch, soluble starch, cassava starch, glutinous starch, lotus root starch and pumpkin starch.
4. The preparation method of the aqueous cement hydration rate regulating material as claimed in claim 1, wherein: the monomer of the water-soluble polymer is one or more of vinyl pyrrolidone, 2-acrylamide-2-methylpropanesulfonic acid, N-vinyl formamide and sodium vinylsulfonate.
5. The preparation method of the aqueous cement hydration rate regulating material as claimed in claim 1, wherein: grafting water-soluble polymer, wherein the using amount of the monomer is 10-40% of the mass of the starch.
6. The preparation method of the aqueous cement hydration rate regulating material as claimed in claim 5, wherein: grafting water-soluble polymer, wherein the using amount of the monomer is 15-25% of the mass of the starch.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811145005.8A CN110963733A (en) | 2018-09-29 | 2018-09-29 | Preparation method of water-based cement hydration rate regulating material |
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| CN201811145005.8A CN110963733A (en) | 2018-09-29 | 2018-09-29 | Preparation method of water-based cement hydration rate regulating material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112724413A (en) * | 2021-01-08 | 2021-04-30 | 西南石油大学 | Preparation method of temperature-sensitive tackifying type suspending agent for well cementation cement slurry |
| CN113429512A (en) * | 2021-06-02 | 2021-09-24 | 宁波锋成先进能源材料研究院有限公司 | Application of water-soluble polymer as curing agent in cement-based material |
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| CN101173027A (en) * | 2007-11-30 | 2008-05-07 | 沈阳建筑大学 | Preparation method and application of starch graft copolymer |
| CN104609769A (en) * | 2015-02-05 | 2015-05-13 | 江苏苏博特新材料股份有限公司 | Cement hydration rate regulating material as well as preparation method and application of cement hydration rate regulating material |
| CN104710131A (en) * | 2015-02-05 | 2015-06-17 | 江苏苏博特新材料股份有限公司 | Cement hydration rate regulation material, and preparation method and application thereof |
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| JPH06305799A (en) * | 1993-04-23 | 1994-11-01 | Nichiden Kagaku Kk | Cement composition |
| JP2003034564A (en) * | 2001-07-18 | 2003-02-07 | Oji Cornstarch Co Ltd | Inhibitor for heat of hydration of cement and manufacturing method of mortar and concrete using it |
| CN101173027A (en) * | 2007-11-30 | 2008-05-07 | 沈阳建筑大学 | Preparation method and application of starch graft copolymer |
| CN104609769A (en) * | 2015-02-05 | 2015-05-13 | 江苏苏博特新材料股份有限公司 | Cement hydration rate regulating material as well as preparation method and application of cement hydration rate regulating material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112724413A (en) * | 2021-01-08 | 2021-04-30 | 西南石油大学 | Preparation method of temperature-sensitive tackifying type suspending agent for well cementation cement slurry |
| CN113429512A (en) * | 2021-06-02 | 2021-09-24 | 宁波锋成先进能源材料研究院有限公司 | Application of water-soluble polymer as curing agent in cement-based material |
| CN113429512B (en) * | 2021-06-02 | 2022-08-02 | 宁波锋成先进能源材料研究院有限公司 | Application of water-soluble polymer as curing agent in cement-based material |
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