CN103739722A - Hydration heat regulating and controlling material as well as preparation method and application thereof - Google Patents
Hydration heat regulating and controlling material as well as preparation method and application thereof Download PDFInfo
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- CN103739722A CN103739722A CN201410010473.XA CN201410010473A CN103739722A CN 103739722 A CN103739722 A CN 103739722A CN 201410010473 A CN201410010473 A CN 201410010473A CN 103739722 A CN103739722 A CN 103739722A
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Abstract
The invention relates to the field of concrete admixtures and particularly relates to a hydration heat regulating and controlling material as well as a preparation method and an application thereof. According to the material with a hydration heat regulating and controlling function, a component is surface cross-linked dextrin prepared by a cross-linking reaction. The invention discloses the hydration heat regulating and controlling material which can greatly regulate and control the hydration speed of cement, reduce the temperature rise of concrete and does not influence the middle-period and post-period strength of the concrete.
Description
Technical field
The present invention relates to concrete admixture field, be specifically related to a kind of hydration heat controlled material and preparation method thereof.
Background technology
Hydrated cementitious can be emitted a large amount of heat, and when in concrete, hydrated cementitious institute liberated heat has little time to shed, concrete internal temperature will raise, and further hydration stops, and concrete temperature can be down to again envrionment temperature; This temperature variation can cause that volume of concrete changes, and under affined condition, can cause concrete cracking, and then affect concrete member weather resistance, security.
In order to reduce the temperature variation in concrete, just need to regulate and control the hydration process of cement, reduce the hydration rate of cement acceleration period as far as possible, make the heat that hydrated cementitious produces not concentrate and discharge, for concrete heat radiation is raced against time, and then reduce the temperature rise that concrete causes because of aquation.
[JP3729340B2] discloses a kind of blended material that is reduced concrete temperature rise by slag and dextrin recombination energy, and the dextrin wherein using is the commercially available dextrin without any modification, its cold water solubility 10%～30%.But open result shows that concrete core temperature reduces amplitude and strength decreased amplitude is proportional, although this blended material plays the effect of cooling, it makes again concrete strength reduce.
[EP1233008A1] discloses a kind of swelling agent material that contains dextrin, adopt commercially available without any modification, cold water solubility lower than 70% dextrin for suppressing hydration heat, disclosed result shows that it makes concrete temperature only reduce by 1 ℃.
[JP4905977B2] is although dextrin has certain hydration heat inhibition, think commercially available without modification, solubleness is that the dextrin of 0-80% has good effect, but it has temperature sensitivity, under the condition of high temperature, its hydration heat inhibition ability can decline, and significantly extended time of coagulation, strength decreased.
Dextrin shows as out the effect similar to traditional small molecules carbohydrate retardant under high volume, and being mainly increases concrete coagulating time, and the ability of the hydration rate of reduction cement weakens on the contrary.
Summary of the invention
For current reported hydration heat, suppress the existing various deficiencies of material: hydration heat suppresses limited in one's ability, easily cause the problems such as strength decreased, serious slow setting.The present invention discloses a kind of hydration heat controlled material, and it can significantly regulate and control hydrated cementitious speed, reduces concrete temperature rise, and does not affect concrete middle and later periods intensity.For addressing the above problem, first object of the present invention is to provide a kind of hydration heat controlled material, and its composition is the surface-crosslinked dextrin of preparing by crosslinking reaction.
Applicant studies discovery, by dextrin surface being carried out to the crosslinked of appropriateness, can not only significantly improve the inhibition ability (higher than uncrosslinked product) of its hydration heat speed, and within the scope of larger volume, can not affect concrete strength and time of coagulation.Can control by the consumption of linking agent degree of crosslinking and the hydration heat rejection of the finished product.
Second object of the present invention is to provide the preparation method of the above-mentioned material with hydration heat adjusting function, a preparation method for hydration heat controlled material, is characterized in that: the raw material of preparing the material of described hydration heat adjusting function comprises dextrin, catalyzer, dispersion medium and linking agent; First described dextrin is dispersed in dispersion medium, then adds linking agent, then regulate pH value to carry out crosslinking reaction, after crosslinking reaction, through separating, be drying to obtain hydration heat controlled material of the present invention; Described linking agent is to have the polyfunctional compound that can react with hydroxyl in described dextrin molecule; Described dispersion medium is water, acetone or tetrahydrofuran (THF); The quality of described dispersion medium and the mass ratio of described dextrin are (9:1)-(0.6:1); The quality of described linking agent is the 0.01-6% of the quality of described dextrin; Described dextrin granular size is 0.1um-800um; Described dextrin number-average molecular weight before crosslinked is 540-100000g/mol.
Applicant's research is found: the initial number-average molecular weight of the hydration heat ability of regulation and control of final surperficial dextrin and surface-crosslinked degree, the size of dextrin, dextrin is relevant, and also can influence each other between rear three, only have between three mutually after coupling, the product obtaining just has optimum effect.Result of study shows: 1), if the cross-linking modified front number-average molecular weight of dextrin is less, it need to select higher degree of crosslinking or large-size, just can make the finished product reach best regulation and control aquation effect; 2) if the cross-linking modified front size of dextrin is less, needs larger number-average molecular weight or select high-crosslinking-degree.
Result of study is also found: 1), along with crosslinked dextrin chi more reduces, its impact on intensity also reduces, but hydration heat inhibition ability is along with the reducing of particle size, and first increases afterwards and reduces.2) along with the increase of dosage of crosslinking agent, hydration heat suppresses ability first to be increased afterwards and reduces; 3) the crosslinked front number-average molecular weight of dextrin is little, and its impact on time of coagulation is larger, but can reduce by increasing degree of crosslinking the negative impact of this aspect.4) crosslinked front dextrin number-average molecular weight is larger, and its hydration heat suppresses ability first to be increased afterwards and reduce, and continue to reduce along with the increase of dextrin number-average molecular weight before crosslinked time of coagulation; 5) unmodified dextrin can make concrete coagulating time significantly extend under high volume, but the inhibition of hydration heat do not promote, and (after condensing, accelerating to rise) on the contrary may decline; Crosslinked dextrin increases along with volume improves hydration heat rejection, also less on impact time of coagulation.6) crosslinked dextrin temperature sensitivity is lower, and under high temperature, hydration heat rejection changes not quite, and less on impact time of coagulation.
Comprehensively above-mentioned, in order to make hydration heat controlled material prepared by the present invention significantly regulate and control hydrated cementitious speed, when reducing concrete temperature rise, do not affect concrete middle and later periods intensity, the number-average molecular weight that add-on, the size of dextrin, the dextrin of the inventor to linking agent in the present invention is initial and the add-on of dispersion agent have been carried out reasonable disposition, just reach effect of the present invention.
The dextrin source that the present invention selects is unrestricted, can through acid or enzymatic hydrolysis, be obtained by various starch.
The present invention is surface modifying method, be that linking agent is only in dextrin particle surface or top layer reaction, therefore system is heterogeneous suspension system, dextrin is present in dispersion medium with the form of solid powder particle, described dispersion medium is water, acetone or tetrahydrofuran (THF), and the quality of described dispersion medium and the mass ratio of described dextrin are (9:1)-(0.6:1).
As preferably, described linking agent is citric acid mixing vinegar acid anhydrides or epoxy chloropropane; In described citric acid mixing vinegar acid anhydrides, the mass ratio of citric acid and acetic anhydride is 1:30; Described pH value is 9-10; The quality of described dispersion medium and the mass ratio of described dextrin are (3:1)-(1.2:1).
As preferably, described linking agent is formaldehyde; Described pH value is 1-3.
As preferably, described dextrin number-average molecular weight before crosslinked is 1000-50000g/mol; The quality of described linking agent is the 0.02-3% of the quality of described dextrin.
As preferably, described dextrin number-average molecular weight before crosslinked is 2000-30000g/mol; The quality of described linking agent is the 0.04-1% of the quality of described dextrin.
As preferably, described dextrin granular size is 1um-300um.
As preferably, described dextrin granular size is 5um-100um.
The 3rd object of the present invention provides the application of a kind of hydration heat controlled material in concrete, the present invention prepare described in there is the material of hydration heat adjusting function addition content be the 0.01-3% of gelling material quality in described concrete.
As preferably, the present invention prepare described in there is the material of hydration heat adjusting function addition content be the 0.05-1.5% of gelling material quality in described concrete.
As preferably, the present invention prepare described in there is the material of hydration heat adjusting function addition content be the 0.1-0.8% of gelling material quality in described concrete.
The invention has the beneficial effects as follows:
(1) the present invention, by dextrin surface being carried out to the crosslinked of appropriateness, can not only significantly improve the inhibition ability of its hydration heat speed, and within the scope of larger volume, can not affect concrete strength and time of coagulation.
(2) preparation method of the present invention is simple, is beneficial to industrialized production.
Embodiment
In order to understand better the present invention, below in conjunction with embodiment, further illustrate content of the present invention, but content of the present invention is not restricted to following embodiment.
Following examples have described in more detail prepared according to the methods of the invention hydration heat controlled material and performance thereof, and these embodiment provide in the mode of explanation, but these embodiment do not limit the scope of the invention.
In the embodiment of the present invention, hydration heat controlled material molecular weight adopts Agilent1200Infinity gel permeation chromatograph to measure.
Adiabatic temperature rise of concrete is used the BY-ATC/JR of Boyuan Science & Technology Development Co. Ltd., Zhoushan City type thermal insulation warming instrument.In embodiment, without special instruction, during thermal insulation warming test, initial temperature is 15 ℃.
In the embodiment of the present invention, cement is used hot 42.5 cement in crossdrift; Water-cement ratio 0.45; Fine aggregate is river sand, apparent density 2.63g/cm3, and fineness modulus is 2.60; Coarse aggregate is that the continuous utmost point of 5～20mm is joined rubble.
Concrete crushing strength is carried out with reference to GB/T50081-2002 < < standard for test methods of mechanical properties of ordinary concrete > >; Concrete coagulating time is carried out with reference to GB/T50080-2002 < < Standard for test methods of properties of ordinary concrete mixture standard > >.
Embodiment 1
1000g number-average molecular weight is 84000g/mol, is of a size of the dextrin of 700um, adds in 2000g water, adds epoxy chloropropane 0.12g, and with NaOH, regulating pH is 10, is warming up to 45 ℃ of reactions 12 hours, is dried after separation to white powder, i.e. dextrin of the present invention.
Embodiment 2
Except used dextrin is of a size of 100um, other is consistent with embodiment 1.
Embodiment 3
Except used dextrin is of a size of 10um, other is consistent with embodiment 1.
Embodiment 4
Except used dextrin is of a size of 0.50um, other is consistent with embodiment 1.
Comparative example 1
The commercially available dextrin without any modification that the solubleness that referenced patent [JP4905977B2] is chosen is 8%.
Comparative example 2
The commercially available dextrin without any modification that the solubleness that referenced patent [JP4905977B2] is chosen is 12%.
Comparative example 3
The commercially available dextrin without any modification that the solubleness that referenced patent [JP4905977B2] is chosen is 48%.
Comparative example 4
The commercially available dextrin without any modification that the solubleness that referenced patent [JP4905977B2] is chosen is 60%.
Comparative example 5
The commercially available dextrin without any modification that the solubleness that referenced patent [JP4905977B2] is chosen is 75%.
Comparative example 6
The commercially available dextrin without any modification that the solubleness that referenced patent [JP4905977B2] is chosen is 82%.
Comparative example 7
The commercially available dextrin without any modification that the solubleness that referenced patent [JP4905977B2] is chosen is 91%.
Comparative example 8
Except not adding linking agent epoxy chloropropane, other is consistent with embodiment 1.
Comparative example 9
Except not adding linking agent epoxy chloropropane, other is consistent with embodiment 1.
Comparative example 10
Except not adding linking agent epoxy chloropropane, other is consistent with embodiment 1.
Comparative example 11
Except not adding linking agent epoxy chloropropane, other is consistent with embodiment 1.
By embodiment 1 to embodiment 4, dextrin prepared by comparative example 1 to comparative example 11 is incorporated in testing method concrete used according to the incorporation in table one, to measure the dextrin mixing, concrete performance is affected.Concrete incorporation and to mix rear concrete test performance as shown in table 1.
The incorporation of the dextrin of table 1 embodiment 1 to 4 and comparative example 1 to 11 preparation in concrete and to coagulation
The impact of soil nature energy
As can be seen from Table 1: 1) add after surface-crosslinked dextrin, Adiabatic temperature rise of concrete lift velocity reduces; 2) the hydration heat inhibition ability of crosslinked rear dextrin is better than there is no crosslinked dextrin, and is better than the commercially available dextrin without modification of several different solubilities of choosing with reference to patent [JP4905977B2]; 3) dextrin can also reduce the impact on time of coagulation after being cross-linked; 4) embodiment 1 to embodiment 4 can find out that crosslinked dextrin chi is less, less on the impact of intensity, but hydration heat suppresses ability along with the reducing of particle size, and first increases afterwards and reduces.
Embodiment 5
1000g number-average molecular weight is 900g/mol, is of a size of the dextrin of 10um, adds in 1500g acetone, adds citric acid mixing vinegar acid anhydrides 50g, and with NaOH, regulating pH is 9, is warming up to 45 ℃ of reactions 8 hours, is dried after separation to white powder.
Embodiment 6
Except used dosage of crosslinking agent is 10g, other is consistent with embodiment 5.
Embodiment 7
Except used dosage of crosslinking agent is 5g, other is consistent with embodiment 5.
Embodiment 8
Except used dosage of crosslinking agent is 0.5g, other is consistent with embodiment 5.
The incorporation of dextrin prepared by table 2 embodiment 5 to 8 and comparative example 1 in concrete and to concrete performance
Impact
Table 2 can be found out: 1) along with the reducing of dosage of crosslinking agent, hydration heat suppresses ability first to be increased afterwards and reduce; 2) embodiment 1 to embodiment 4 in associative list 1, can find out that the crosslinked front number-average molecular weight of dextrin is little, and its impact on time of coagulation is larger, but can reduce by increasing degree of crosslinking the negative impact of this aspect.
Embodiment 9
1000g number-average molecular weight is 3200g/mol, is of a size of the dextrin of 15um, adds in 1000g tetrahydrofuran (THF), adds formaldehyde 1g, and with HCl, regulating pH is 2, is warming up to 45 ℃ of reactions 5 hours, is dried after separation to white powder.
Embodiment 10
Except used dextrin number-average molecular weight is 8500 for g/mol, other is consistent with embodiment 9.
Embodiment 11
Except used dextrin number-average molecular weight is 21000 for g/mol, other is consistent with embodiment 9.
Comparative example 13
Except the raw material that uses before modification for W-Gum but not dextrin (starch number-average molecular weight average out to 1200000 used, other is consistent with embodiment 9.
Comparative example 14
Directly add the concrete of W-Gum.
Comparative example 15
Except not adding linking agent formaldehyde, other is consistent with embodiment 9.
Comparative example 16
Except not adding linking agent formaldehyde, other is consistent with embodiment 10.
Comparative example 17
Except not adding linking agent formaldehyde, other is consistent with embodiment 11.
Dextrin the mixing in concrete of table 3 embodiment 9 to 11 and comparative example 1 and comparative example 12 to 16 preparations
Enter amount and the impact on concrete performance thereof
Table 3 can be found out: 1), along with dextrin number-average molecular weight before crosslinked increases, hydration heat suppresses ability first to be increased afterwards and reduce, and continued to reduce time of coagulation along with the increase of dextrin number-average molecular weight before crosslinked; 2) surface-crosslinked dextrin hydration heat inhibition ability is greater than does not have crosslinked dextrin.
Comparative example 17
Except the volume of preparing dextrin is increased to 0.3 by 0.15%, other is identical with comparative example 15.
Comparative example 18
Except the volume of preparing dextrin is increased to 0.8 by 0.15%, other is identical with comparative example 15.
Embodiment 12
Except the volume of preparing dextrin is increased to 0.3 by 0.15%, other is identical with embodiment 10.
Embodiment 13
Except the volume of preparing dextrin is increased to 0.8 by 0.15%, other is identical with embodiment 10.
Table 4 embodiment 10, embodiment 12, embodiment 13 and comparative example 1, comparative example 14, comparative example 17 and
Dextrin prepared by comparative example 18 incorporation in concrete and the impact on concrete performance thereof
Table 4 can be found out: 1) unmodified dextrin can make concrete coagulating time significantly extend under high volume, but the inhibition of hydration heat do not promote, and (after condensing, accelerating to rise) on the contrary may decline; Crosslinked dextrin increases along with volume improves hydration heat rejection, and time of coagulation, amplification was also much smaller than uncrosslinked dextrin.
Comparative example-19
Except Adiabatic temperature rise of concrete test initial temperature is increased to 35 ℃ by original 15 ℃, other is identical with comparative example 15.
Embodiment-14
Except Adiabatic temperature rise of concrete test initial temperature is increased to 35 ℃ by original 15 ℃, other is identical with embodiment 10.
Paste prepared by table 5 embodiment 10, embodiment 14 and comparative example 1, comparative example 15 and comparative example 19
The incorporation of essence in concrete and the impact on concrete performance thereof
Table 5 can be found out: crosslinked dextrin temperature sensitivity is lower, and under high temperature, hydration heat rejection changes not quite, and affects hardly time of coagulation.
Claims (11)
1. a hydration heat controlled material, is characterized in that: its composition is the surface-crosslinked dextrin of preparing by crosslinking reaction.
2. a preparation method for hydration heat controlled material, is characterized in that: the raw material of preparing the material of described hydration heat adjusting function comprises dextrin, catalyzer, dispersion medium and linking agent; First described dextrin is dispersed in dispersion medium, then adds linking agent, then regulate pH value to carry out crosslinking reaction, after crosslinking reaction, through separating, be drying to obtain hydration heat controlled material of the present invention; Described linking agent is to have the polyfunctional compound that can react with hydroxyl in described dextrin molecule; Described dispersion medium is water, acetone or tetrahydrofuran (THF); The quality of described dispersion medium and the mass ratio of described dextrin are (9:1)-(0.6:1); The quality of described linking agent is the 0.01-6% of the quality of described dextrin; Described dextrin granular size is 0.1um-800um; Described dextrin number-average molecular weight before crosslinked is 540-100000g/mol.
3. a kind of preparation method of hydration heat controlled material as claimed in claim 2, is characterized in that: described linking agent is citric acid mixing vinegar acid anhydrides or epoxy chloropropane; In described citric acid mixing vinegar acid anhydrides, the mass ratio of citric acid and acetic anhydride is 1:30; Described pH value is 9-10; The quality of described dispersion medium and the mass ratio of described dextrin are (3:1)-(1.2:1).
4. a kind of preparation method of hydration heat controlled material as claimed in claim 2, is characterized in that: described linking agent is formaldehyde; Described pH value is 1-3.
5. a kind of hydration heat controlled material as described in claim 3 or 4 any one, is characterized in that: described dextrin number-average molecular weight before crosslinked is 1000-50000g/mol; The quality of described linking agent is the 0.02-3% of the quality of described dextrin.
6. a kind of hydration heat controlled material as claimed in claim 5, is characterized in that: described dextrin number-average molecular weight before crosslinked is 2000-30000g/mol; The quality of described linking agent is the 0.04-1% of the quality of described dextrin.
7. a kind of preparation method of hydration heat controlled material as claimed in claim 6, is characterized in that: described dextrin granular size is 1um-300um.
8. a kind of preparation method of hydration heat controlled material as claimed in claim 7, is characterized in that: described dextrin granular size is 5um-100um.
9. as claim 1,2,3,4,6,7, the application of a kind of hydration heat controlled material in concrete described in 8 any one, is characterized in that: the present invention prepare described in there is the material of hydration heat adjusting function addition content be the 0.01-3% of gelling material quality in described concrete.
10. the application of a kind of hydration heat controlled material in concrete as claimed in claim 9, is characterized in that: the present invention prepare described in there is the material of hydration heat adjusting function addition content be the 0.05-1.5% of gelling material quality in described concrete.
11. application of a kind of hydration heat controlled material in concrete as claimed in claim 10, is characterized in that: the present invention prepare described in there is the material of hydration heat adjusting function addition content be the 0.1-0.8% of gelling material quality in described concrete.
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| CN104592403A (en) * | 2015-02-05 | 2015-05-06 | 江苏苏博特新材料股份有限公司 | Hydration heat regulating agent and preparation method and application thereof |
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| CN104609766A (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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| CN104610503A (en) * | 2015-02-05 | 2015-05-13 | 江苏苏博特新材料股份有限公司 | Crosslinked hydration heat regulating agent as well as preparation method and application of crosslinked hydration heat regulating agent |
| CN104592403A (en) * | 2015-02-05 | 2015-05-06 | 江苏苏博特新材料股份有限公司 | Hydration heat regulating agent and preparation method and application thereof |
| CN104628297A (en) * | 2015-02-05 | 2015-05-20 | 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 thereof |
| CN104609766A (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 |
| CN104710132A (en) * | 2015-02-05 | 2015-06-17 | 江苏苏博特新材料股份有限公司 | Cement hydration rate regulating and control material and preparation method and application thereof |
| CN106093304A (en) * | 2016-06-08 | 2016-11-09 | 江苏苏博特新材料股份有限公司 | A kind of method of testing characterizing heat of hydration controlled material temperature control effect |
| CN106093304B (en) * | 2016-06-08 | 2018-05-04 | 江苏苏博特新材料股份有限公司 | A kind of test method for characterizing heat of hydration controlled material temperature control effect |
| CN108341611A (en) * | 2018-04-16 | 2018-07-31 | 广东水电二局股份有限公司 | A kind of heat of hydration regulation and control composition and the preparation method and application thereof |
| CN109680717A (en) * | 2019-01-30 | 2019-04-26 | 武汉市市政建设集团有限公司 | A kind of Underground Rail Transit sidewall structure cracking-proof construction method |
| CN109680717B (en) * | 2019-01-30 | 2021-03-16 | 武汉市市政建设集团有限公司 | Anti-crack construction method for side wall structure of underground rail transit |
| CN109776022A (en) * | 2019-03-07 | 2019-05-21 | 东南大学 | The compound controllable heat of hydration cement-based material of one kind and its application |
| CN109776022B (en) * | 2019-03-07 | 2021-06-11 | 东南大学 | Composite controllable hydration cement-based material and application thereof |
| CN112551935A (en) * | 2019-09-25 | 2021-03-26 | 中路高科交通检测检验认证有限公司 | Concrete hydration heat inhibiting material and preparation method thereof |
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