CN104710131B - Cement hydration rate regulation material, and preparation method and application thereof - Google Patents
Cement hydration rate regulation material, and preparation method and application thereof Download PDFInfo
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- CN104710131B CN104710131B CN201510060171.8A CN201510060171A CN104710131B CN 104710131 B CN104710131 B CN 104710131B CN 201510060171 A CN201510060171 A CN 201510060171A CN 104710131 B CN104710131 B CN 104710131B
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Abstract
The invention provides a cement hydration rate regulation material. The cement hydration rate regulation material is water-insoluble polymer wrapped modified dextrin, wherein a mass ratio of the water-insoluble polymer to dextrin is (0.05-10):(90-99.95). The cement hydration rate regulation material has the advantages of simple preparation technology, low cost, and greatly improved cement hydration rate regulation performance. The influence of the hydration rate regulation material on cement hydration is different from that of a traditional micro-molecular retarder, the regulation material has small even no influence on the induction period of hydration, but greatly reduces hydration rate in the acceleration period and the deceleration period, and the traditional micro-molecular retarder prolongs the induction period of cement hydration, and basically has no influence on the hydration rate in the acceleration period and the deceleration period of cement hydration.
Description
Technical field
The invention belongs to concrete admixture field is and in particular to a kind of hydrated cementitious speed controlled material and its preparation side
Method and application.
Background technology
The Crack Control problem of concrete is one of critically important problem in architectural engineering, and wherein thermal cracking is
Common crack form.Hydrated cementitious can release substantial amounts of heat, when in concrete, hydrated cementitious institute liberated heat has little time to dissipate
When going out, concrete internal temperature will raise, and further hydration stops, and concrete temperature can be down to ambient temperature again；This temperature
Degree change can cause volume of concrete to change, under the conditions of affined, when the tension that temperature deformation is formed exceedes concrete
During tensile strength, may result in the formation of thermal cracking.
In order to reduce the temperature change in concrete it is necessary to the hydration process of regulation and control cement, reduce cement as far as possible and accelerate
The hydration rate of phase, so that heat produced by hydrated cementitious must not concentrate release, is that concrete radiating is raced against time, and then drops
The temperature rise that low concrete causes because of aquation, reduces the temperature stress of inside concrete, and then reduces cracking risk.
Patent JP3729340B2 discloses a kind of mixing material being reduced concrete temperature rise by slag and dextrin recombination energy, its
Used in dextrin be commercially available no any modification dextrin, its cold water solubility 10～30%；However, open result shows
Show：The central temperature of concrete reduces amplitude and intensity decreases amplitude is proportional, although that is, this mixing material plays the work of cooling
With, but it makes concrete strength reduce again.
Patent EP1233008A1 discloses a kind of expansion agent material containing dextrin, using commercially available no any modification,
Cold water solubility is used for suppressing the heat of hydration less than 70% dextrin, and disclosed result shows it so that concrete temperature reduced by only 1
DEG C, effect on driving birds is not good.
Patent CN201410010473 discloses a kind of heat of hydration controlled material and preparation method and application：It uses
Surface crosslinking agent dextrin, after result display crosslinking, effect has a certain upgrade, but the complex process and time is longer.
Patent CN201410009447 discloses a kind of moderate-heat portland cement Hydration controlled material, its by dextrin,
Modified dextrins and Oleic acid composition, the optimum proportioning of disclosed result display can reduce hydrated cementitious maximum rate peak value 66.3%,
But it prepared also more complicated.
In sum, although existing patent documentation is mentioned dextrin and had certain hydration rate adjusting function, dextrin is to form sediment
The intermediate product of powder hydrolysis, species is various, and not every dextrin all has outstanding aquation adjusting function；Published at present
In patent or document, the material preparation process with aquation adjusting function was also loaded down with trivial details it is therefore necessary to prepared by exploitation one kind
Journey process is simple, environmental protection and the excellent hydrated cementitious speed controlled material of final performance.
Content of the invention
Goal of the invention：In order to overcome the above-mentioned deficiencies of the prior art, it is an object of the invention to provide a kind of hydrated cementitious
Speed controlled material.
Technical scheme：
Applicant is found by numerous studies：Dextrin can effectively reduce hydrated cementitious speed essential reason：Dextrin is in water
Mud particle surface forms one layer of adsorption layer, and this layer of adsorption layer reduces the speed by export-oriented cement granules internal migration for the moisture, enter
And reduce the hydration rate of cement；And dextrin easily hydrolyzes in the basic conditions, generate the hydroxy acid of small molecule, this makes to inhale
Attached layer is destroyed, and then affects its aquation performance of control, and the micromolecular hydroxyl acid that dextrin degradation is formed also causes cement water
Change induction period significantly to extend.The present invention proposes using relatively hydrophobic polymerization to dextrin is carried out with a certain degree of parcel, reduces paste
Essence and the contact area of cement alkalescence hole solution, reduce the ratio that dextrin is degraded in aquation induction period, and then reduce dextrin pair
The impact of aquation induction period, can also lift the performance improving dextrin simultaneously.
A kind of hydrated cementitious speed controlled material that the present invention provides, is the modified dextrin of non-soluble polymer parcel.
Preferably, described dextrin number-average molecular weight is 1000～90000g/mol；Preferably, the equal molecule of described dextrin number
Measure as 2000～60000g/mol；It is highly preferred that described dextrin number-average molecular weight is 5000～30000g/mol.The present invention can make
Use various dextrin, its source is unrestricted, can be obtained through acid or enzymatic hydrolysis by various starch, preparation method refers to
Documents and materials disclosed in this area；The cold water-soluble of dextrin is unrestricted, can be the white dextrin of incomplete cold water solubless,
Can be the yellow starch gum or maltodextrin being completely dissolved.
As another kind preferably, described non-soluble polymer kind is unrestricted, but preferably easy film forming polymer, more excellent
Select ethylene-vinyl acetate copolymer；The number-average molecular weight of described ethylene-vinyl acetate copolymer is 1000-500000g/
Mol, vinyl acetate content is 5-60mol%.
As another kind of preferred, the mass ratio (0.05-10) of described non-soluble polymer and dextrin：(90-99.95)；
Preferably, the mass fraction of described non-soluble polymer is 0.05-10%.
The preparation of hydrated cementitious speed controlled material of the present invention adopts following methods：By non-soluble polymer with suitable
Organic solvent dissolves, and adds the dextrin mix homogeneously of metering, removes organic solvent, obtains required aquation controlled material.
Present invention also offers application in concrete for the above-mentioned hydrated cementitious speed controlled material, described hydrated cementitious speed
The volume (with respect to consumption of glue material) of rate controlled material is 0.1-2%, more preferably 0.15-1%.
Beneficial effect：The hydrated cementitious speed controlled material preparation process is simple of present invention offer, with low cost, suitable work
Industry metaplasia is produced, and it has very big lifting to hydrated cementitious speed performance of control with respect to prior art.Meanwhile, this hydration rate is adjusted
The impact of the control aquation to cement for the material is different from traditional small molecule retarder, and this controlled material affects relatively on the induction period of aquation
Little but can significantly reduce the hydration rate of accelerated period and deceleration phase even without impact, and traditional small molecule retarder master
If extending hydrated cementitious induction period, and substantially no (see Fig. 1) is affected to the hydration rate of hydrated cementitious accelerated period and deceleration phase.
Brief description
Fig. 1 is the hydrated cementitious speed controlled material of the present invention impact different to hydrated cementitious from conventional set retarder (sucrose)
Rule (test of TAM AIR isothermal calorimeter obtains)
Specific embodiment
Following examples described in more detail hydrated cementitious speed controlled material prepared according to the methods of the invention and
Its performance, and these embodiments are given by way of illustration, but these embodiments do not limit the scope of the invention.
In the embodiment of the present invention, molecular weight adopts Agilent 1200 Infinity chromatograph of gel permeation to measure.
The monitoring of hydrated cementitious exothermic process adopts U.S. TA company's T AM AIR isothermal calorimeter, and test temperature is 20 DEG C, surveys
Part of having a try be net starch, water-cement ratio is 0.4, hydrated cementitious speed controlled material add the material that percentage ratio is with respect to glue material.With
Maximum heatrelease rate peak value reduces amplitude as the criterion of aquation controlled material performance of the present invention, heat release speed under the same terms
Rate peak value reduction amplitude is more big, shows that hydrated cementitious speed controlled material performance is better, is more avoided that the concentration of hydrated cementitious is put
Heat.
Concrete crushing strength is with reference to GB/T50081-2002《Standard for test methods of mechanical properties of ordinary concrete》Execution；
Concrete coagulating time is with reference to GB/T50080-2002《Standard for test methods of properties of ordinary concrete mixture standard》Execution.
In the embodiment of the present invention, as shown in table 1 using concrete mix.Wherein, cement uses Carnis Rapanae thomasianae 42.5 cement；One
Level flyash；Fine aggregate is river sand, apparent density 2.63g/cm3, and modulus of fineness is 2.60；Coarse aggregate is the continuous pole of 5～20mm
Join rubble.
Table 1 concrete foundation match ratio (kg/m3)
Embodiment 1
Number-average molecular weight is the dextrin of 1000g/mol, and addition number-average molecular weight is 30000g/mol, vinyl acetate content
In the dichloromethane solution of the ethylene-vinyl acetate copolymer for 5%, the matter of dextrin and ethylene-vinyl acetate copolymer
Amount ratio is 99:1, remove methylene chloride, gained solid drying after stirring 5min, pulverize the aquation regulation and control required for obtaining
Material.
Embodiment 2
Number-average molecular weight is the dextrin of 2000g/mol, and addition number-average molecular weight is 30000g/mol, vinyl acetate content
In the dichloromethane solution of the ethylene-vinyl acetate copolymer for 20%, the matter of dextrin and ethylene-vinyl acetate copolymer
Amount ratio is 99:1, remove methylene chloride, gained solid drying after stirring 5min, pulverize the aquation regulation and control required for obtaining
Material.
Embodiment 3
Number-average molecular weight is the dextrin of 5000g/mol, and addition number-average molecular weight is 30000g/mol, vinyl acetate content
In the dichloromethane solution of the ethylene-vinyl acetate copolymer for 30%, the matter of dextrin and ethylene-vinyl acetate copolymer
Amount ratio is 99:1, remove methylene chloride, gained solid drying after stirring 5min, pulverize the aquation regulation and control required for obtaining
Material.
Embodiment 4
Number-average molecular weight is the dextrin of 15000g/mol, and addition number-average molecular weight is 30000g/mol, and vinylacetate contains
Measure in the dichloromethane solution of the ethylene-vinyl acetate copolymer for 30%, dextrin and ethylene-vinyl acetate copolymer
Mass ratio is 99:1, remove methylene chloride, gained solid drying after stirring 5min, pulverize the aquation required for obtaining and adjust
Control material.
Embodiment 5
Number-average molecular weight is the dextrin of 30000g/mol, and addition number-average molecular weight is 30000g/mol, and vinylacetate contains
Measure in the ethanol solution of the ethylene-vinyl acetate copolymer for 40%, the quality of dextrin and ethylene-vinyl acetate copolymer
Than for 99:1, remove etoh solvent, gained solid drying after stirring 5min, pulverize the aquation controlled material required for obtaining.
Embodiment 6
Number-average molecular weight is the dextrin of 60000g/mol, and addition number-average molecular weight is 30000g/mol, and vinylacetate contains
Measure in the ethanol solution of the ethylene-vinyl acetate copolymer for 50%, the quality of dextrin and ethylene-vinyl acetate copolymer
Than for 99:1, remove etoh solvent, gained solid drying after stirring 5min, pulverize the aquation controlled material required for obtaining.
Embodiment 7
Number-average molecular weight is the dextrin of 90000g/mol, and addition number-average molecular weight is 30000g/mol, and vinylacetate contains
Measure in the ethanol solution of the ethylene-vinyl acetate copolymer for 40%, the quality of dextrin and ethylene-vinyl acetate copolymer
Than for 99:1, remove etoh solvent, gained solid drying after stirring 5min, pulverize the aquation controlled material required for obtaining.
Comparative example 1
Without the net slurry of any additive, concrete.
Comparative example 2
Number-average molecular weight is the dextrin of 1000g/mol is 30000g/mol with number-average molecular weight, and vinyl acetate content is
5% ethylene-vinyl acetate copolymer is with mass ratio for 99:1 direct physics is combined the mixture obtaining.
Comparative example 3
Number-average molecular weight is the dextrin of 2000g/mol is 30000g/mol with number-average molecular weight, and vinyl acetate content is
20% ethylene-vinyl acetate copolymer is with mass ratio for 99:1 direct physics is combined the mixture obtaining.
Comparative example 4
Number-average molecular weight is the dextrin of 5000g/mol is 30000g/mol with number-average molecular weight, and vinyl acetate content is
30% ethylene-vinyl acetate copolymer is with mass ratio for 99:1 direct physics is combined the mixture obtaining.
Comparative example 5
Number-average molecular weight is the dextrin of 15000g/mol is 30000g/mol with number-average molecular weight, and vinyl acetate content is
40% ethylene-vinyl acetate copolymer is with mass ratio for 99:1 direct physics is combined the mixture obtaining.
Comparative example 6
Number-average molecular weight is the dextrin of 30000g/mol is 30000g/mol with number-average molecular weight, and vinyl acetate content is
50% ethylene-vinyl acetate copolymer is with mass ratio for 99:1 direct physics is combined the mixture obtaining.
Comparative example 7
Number-average molecular weight is the dextrin of 60000g/mol is 30000g/mol with number-average molecular weight, and vinyl acetate content is
40% ethylene-vinyl acetate copolymer is with mass ratio for 99:1 direct physics is combined the mixture obtaining.
Comparative example 8
Number-average molecular weight is the dextrin of 90000g/mol is 30000g/mol with number-average molecular weight, and vinyl acetate content is
40% ethylene-vinyl acetate copolymer is with mass ratio for 99:1 direct physics is combined the mixture obtaining.
Comparative example 9
【CN201410009447】Disclosed result 0.2% volume, aquation maximum rate peak value reduces by 62.4%.
The hydrated cementitious speed controlled material of embodiment 1 to 7 is added in concrete, the results are shown in Table 2.
Table 2 concrete performance
In table, result be can be seen that the hydration rate controlled material being prepared by the method that the present invention provides and can reduce
Aquation maximum rate peak value more than 75%, better than published result at present；It is only blending dextrin and macromolecule organic, its
Effect is limited, the product preparing far below the method being provided by the present invention.
Embodiment 8
Number-average molecular weight is the dextrin of 26000g/mol, and addition number-average molecular weight is 8000g/mol, vinyl acetate content
In the dichloromethane solution of the ethylene-vinyl acetate copolymer for 20%, the matter of dextrin and ethylene-vinyl acetate copolymer
Amount ratio is 92:8, remove methylene chloride, gained solid drying after stirring 5min, pulverize the aquation regulation and control required for obtaining
Material.
Embodiment 9
Number-average molecular weight is the dextrin of 26000g/mol, and addition number-average molecular weight is 100000g/mol, and vinylacetate contains
Measure in the dichloromethane solution of the ethylene-vinyl acetate copolymer for 20%, dextrin and ethylene-vinyl acetate copolymer
Mass ratio is 95:5, remove methylene chloride, gained solid drying after stirring 5min, pulverize the aquation required for obtaining and adjust
Control material.
Embodiment 10
Number-average molecular weight is the dextrin of 26000g/mol, and addition number-average molecular weight is 250000g/mol, and vinylacetate contains
Measure in the dichloromethane solution of the ethylene-vinyl acetate copolymer for 20%, dextrin and ethylene-vinyl acetate copolymer
Mass ratio is 99:1, remove methylene chloride, gained solid drying after stirring 5min, pulverize the aquation required for obtaining and adjust
Control material.
Embodiment 11
Number-average molecular weight is the dextrin of 26000g/mol, and addition number-average molecular weight is 350000g/mol, and vinylacetate contains
Measure in the tetrahydrofuran solution of the ethylene-vinyl acetate copolymer for 20%, dextrin and ethylene-vinyl acetate copolymer
Mass ratio is 99.5:0.5, remove solvents tetrahydrofurane, gained solid drying after stirring 5min, pulverize the water required for obtaining
Change controlled material.
Embodiment 12
Number-average molecular weight is the dextrin of 26000g/mol, and addition number-average molecular weight is 450000g/mol, and vinylacetate contains
Measure in the ethanol solution of the ethylene-vinyl acetate copolymer for 20%, the quality of dextrin and ethylene-vinyl acetate copolymer
Than for 99.9:0.1, remove etoh solvent, gained solid drying after stirring 5min, pulverize the aquation regulation and control material required for obtaining
Material.
The hydrated cementitious speed controlled material of embodiment 8 to 12 is added in concrete, the results are shown in Table 3.
Table 3 concrete performance
Table 3 can be seen that：The hydration rate controlled material being prepared by the method that the present invention provides can reduce aquation
Maximum rate peak value more than 75%, better than published result at present.
Embodiment 13
Number-average molecular weight is the dextrin of 90000g/mol, and addition number-average molecular weight is 500000g/mol, and vinylacetate contains
Measure in the dichloromethane solution of the ethylene-vinyl acetate copolymer for 60%, dextrin and ethylene-vinyl acetate copolymer
Mass ratio is 99.95:0.05, remove methylene chloride, gained solid drying after stirring 5min, pulverize required for obtaining
Aquation controlled material.
Embodiment 14
Number-average molecular weight is the dextrin of 60000g/mol, and addition number-average molecular weight is 100000g/mol, and vinylacetate contains
Measure in the dichloromethane solution of the ethylene-vinyl acetate copolymer for 40%, dextrin and ethylene-vinyl acetate copolymer
Mass ratio is 95:5, remove methylene chloride, gained solid drying after stirring 5min, pulverize the aquation required for obtaining and adjust
Control material.
Embodiment 15
Number-average molecular weight is the dextrin of 30000g/mol, and addition number-average molecular weight is 10000g/mol, and vinylacetate contains
Measure in the dichloromethane solution of the ethylene-vinyl acetate copolymer for 20%, dextrin and ethylene-vinyl acetate copolymer
Mass ratio is 94:6, remove methylene chloride, gained solid drying after stirring 5min, pulverize the aquation required for obtaining and adjust
Control material.
Embodiment 16
Number-average molecular weight is the dextrin of 10000g/mol, and addition number-average molecular weight is 1000g/mol, vinyl acetate content
In the dichloromethane solution of the ethylene-vinyl acetate copolymer for 5%, the matter of dextrin and ethylene-vinyl acetate copolymer
Amount ratio is 90:10, remove methylene chloride, gained solid drying after stirring 5min, pulverize the aquation required for obtaining and adjust
Control material.
The hydrated cementitious speed controlled material of embodiment 13 to 16 is added in concrete, the results are shown in Table 4.
Table 4 concrete performance
Claims (6)
1. a kind of hydrated cementitious speed controlled material it is characterised in that：Described hydrated cementitious speed controlled material is water-insoluble
The modified dextrin of polymer wrapped；Described dextrin number-average molecular weight is 1000～90000g/mol；Described non-soluble polymer
For easy film forming polymer, selected from ethylene-vinyl acetate copolymer, it is (0.05-10) with the mass ratio of dextrin：(90-
99.95).
2. a kind of hydrated cementitious speed controlled material according to claim 1 it is characterised in that：The equal molecule of described dextrin number
Amount is in 2000～60000g/mol.
3. a kind of hydrated cementitious speed controlled material according to claim 1 it is characterised in that：The equal molecule of described dextrin number
Amount is in 5000～30000g/mol.
4. a kind of hydrated cementitious speed controlled material according to claim 1 it is characterised in that：Described ethyl vinyl acetate second
The number-average molecular weight of enoate copolymer is 1000-500000g/mol, and vinyl acetate content is 5-60mol%.
5. application in concrete for the hydrated cementitious speed controlled material described in any one of claim 1-4 it is characterised in that：
The volume of described hydrated cementitious speed controlled material is 0.1-2%.
6. application in concrete for the hydrated cementitious speed controlled material according to claim 5 it is characterised in that：Described
The volume of hydrated cementitious speed controlled material is 0.15-1%.
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| CN108585572B (en) * | 2018-02-05 | 2019-12-31 | 武汉优城科技有限公司 | Polymer surface modified calcium sulphoaluminate expanding agent and preparation method thereof |
| CN110963733A (en) * | 2018-09-29 | 2020-04-07 | 镇江苏博特新材料有限公司 | Preparation method of water-based cement hydration rate regulating material |
| CN112551930B (en) * | 2020-12-11 | 2021-08-17 | 河南理工大学 | Coated excitant for alkali slag cement and preparation method thereof |
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| JP3343428B2 (en) * | 1993-12-22 | 2002-11-11 | 太平洋セメント株式会社 | Hydration heat inhibitor for cement |
| JP4727020B2 (en) * | 1999-03-29 | 2011-07-20 | 電気化学工業株式会社 | Cement composition |
| WO2013087391A1 (en) * | 2011-12-16 | 2013-06-20 | Construction Research & Technology Gmbh | Shellac-coated particles of active ingredients with controlled release properties at high ph-values, process for their manufacture and use thereof |
| CN103833259B (en) * | 2014-01-09 | 2015-08-19 | 江苏苏博特新材料股份有限公司 | A kind of moderate-heat portland cement Hydration controlled material |
| CN103739722B (en) * | 2014-01-10 | 2016-03-23 | 江苏苏博特新材料股份有限公司 | A kind of hydration heat controlled material and preparation method thereof and application |
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