CN103435317A - Compound expanding agent for inhibiting temperature rising in early stage and promoting hydration in later stage and preparation method thereof - Google Patents
Compound expanding agent for inhibiting temperature rising in early stage and promoting hydration in later stage and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of building material, and particularly relates to a compound expanding agent for inhibiting temperature rising in the early stage and promoting hydration in the later stage. The compound expanding agent comprises the following raw materials by weight: 10 to 30 % of calcium oxide, 28 to 43 % of sulphate aluminium cement clinker, 25 to 40 % of anhydrite, 5 to 15 % of magnesium oxide, 0.3 to 0.5 % of boric acid, 1 to 1.5 % of zinc sulfate and 0.2 to 0.5 % of ICA. The compound expanding agent has the advantages of high early stage expanding capacity, sustainable expansion and long expanding stable period, can effectively compensate self-constriction and drying shrinkage of concrete, enables the synergetic development of the volume expansion and the strength increase of concrete, and is very suitable for being applied to steel pipe concrete and mass concrete.
Description
Technical field
The invention belongs to building material field, be specifically related to composite expanding agent of a kind of early stage inhibition temperature rise later stage promotion aquation and preparation method thereof.
Background technology
Due to the continuous progress that modern material prepares level and building construction technology, the construction of super high rise building and the large steel pipe arch bridge across footpath more and more is subject to people's favor, so the application of the engineering of concrete filled steel tube and mass concrete is very frequent.Yet current steel tube concrete soil material, the common intensity grade is high, and gel material content is large, and water-cement ratio is low, and airtight in steel pipe, can't carry out in the environment of exchange of moisture with the external world, concrete shrinkage is large, and inner self-desiccation is rapid, and the aquation of swelling agent is limited large, be difficult to continual and steady expansion, be easy to the phenomenon that causes concrete and steel pipe " to come to nothing ", make the globality of structure impaired, affect greatly its bearing capacity and work-ing life; And in mass concrete, the heat of hydrated cementitious is difficult for shedding, the aquation temperature rise is large, makes the interior table of the concrete temperature difference large, is easy to cause inhomogeneous temperature deformation and thermal stress, causes thus the generation of thermal cracking, affects its weather resistance.Although mix swelling agent in mass concrete, can compensate its self-constriction and dry shrinkage, the general early hydration of swelling agent is very fast, and heat release is rapid, is unfavorable for controlling its aquation temperature rise, to avoid the appearance of thermal cracking.Therefore need prepare a kind of early expansion can large, sustainable expansion, expansion stable period is long, can suppress the aquation temperature rise, and the spontaneous water of releasing of later stage energy, regulate ambient humidity, guarantee that hydration swelling continues the interior maintenance composite expanding agent carried out, and make it in concrete filled steel tube and mass concrete engineering, obtain applications well.
Summary of the invention
The object of the present invention is to provide a kind of early stage inhibition temperature rise later stage to promote composite expanding agent of aquation and preparation method thereof.
To achieve these goals, technical scheme of the present invention is:
A kind of early stage inhibition temperature rise later stage promotes the composite expanding agent of aquation, by calcium oxide, sulphoaluminate cement clinker, anhydrite, magnesium oxide, boric acid, zinc sulfate and ICA, formed, the mass percent of each component is: calcium oxide 10～30%, sulphoaluminate cement clinker 28～43%, anhydrite 25～40%, magnesium oxide 5～15%, boric acid 0.3～0.5%, zinc sulfate 1～1.5%, ICA0.2～0.5%.
In such scheme, described calcium oxide is light-burned calcium oxide, be by calcite after fragmentation, through 900～1100 ℃ of high-temperature calcinations, form.
In such scheme, described sulphoaluminate cement clinker is by anhydrous calcium sulphoaluminate
tetracalcium aluminoferrite (C
4aF) and Dicalcium Phosphate (Feed Grade) (C
2s) form, the mass percent of each component is:
c
4aF:3.5～8%, C
2s:18.5～37.5%.
In such scheme, described anhydrite is natural or artificial anhydrite.
In such scheme, described magnesium oxide was burned magnesium oxide, was to be formed through 1300～1400 ℃ of high-temperature calcinations by magnesite its specific surface area>=450m
2/ kg, the measuring method of specific surface area is: " GB/T8074-2008 Method of determination for specific surface of cement (Bo Shi method) ".
In such scheme, described boric acid is the white powder crystallization, and satiny feel is arranged, odorless, and density is about 1.43g/cm
3.
In such scheme, described zinc sulfate is white powder, odorlessness, and puckery, density is about 1.96g/cm
3.
In such scheme, described ICA is that tapioca (flour) is polymer-modified, its structural formula as shown in the formula (I):
In such scheme, the preparation method of described ICA comprises the steps:
(1) starch pasting: take 1～4 portion of tapioca (flour) of weight part and be dissolved in distilled water and stir, then join in reactor, heating gelatinization;
(2) free radical causes: take ceric ammonium nitrate and ammonium persulphate totally 0.1～0.5 weight part be dissolved in distilled water, ceric ammonium nitrate wherein: the mass ratio of ammonium persulphate is 1:9, after stirring, joins in the described reactor of step (1);
(3) graft copolymerization: take respectively the two Methacrylamides of 0.1～10 weight parts monomers acrylamide and 0.01～0.05 weight part, water-soluble and stir, obtain monomer solution; Monomer solution need be added drop-wise in the described reactor of step (1) after the described radical initiation reaction 10min of step (2) again, and the time for adding of controlling monomer solution under 50～80 ℃ of conditions is 0.5～1h;
(4) composite crosslinking: get the 2-acrylamide-2-methyl propane sulfonic and be dissolved in distilled water and obtain 2-acrylamide-2-methyl propane sulfonic solution, wherein the mass ratio of the described monomer acrylamide of 2-acrylamide-2-methyl propane sulfonic and step (3) is 1:1～1:9; Get a certain amount of water glass solution, make developer with phenolphthalein, drip 2-acrylamide-2-methyl propane sulfonic solution with water glass solution, in 2-acrylamide-2-methyl propane sulfonic solution, the color of phenolphthalein is from the colourless redness that changes into gradually, and, when redness is no longer taken off, obtain pre-polysilicic acid sol azury; The pre-polysilicic acid sol of gained is dropped in the described reactor of step (1), the mechanical stirring rotating speed is 80～100r/min, temperature of reaction is 50～80 ℃, and the reaction times is 2.5～3h, and reaction obtains colourless spawn or contains the strong solution of colourless spawn after finishing;
(5) hydrolysis: NaOH is water-soluble, regulate pH value 10～12, join in the described reactor of step (1), hydrolysis obtains crude product;
(6) above-mentioned crude product, after suction filtration, is soaked with ethanol and acetone, and washing, obtain pure products;
(7) above-mentioned pure products is dried to constant weight, after broken and grinding, obtain the ICA powder.
In such scheme, water-intake rate >=80g/g of described ICA, release water rate >=80wt%, water-intake rate and release the water rate and measure with reference to the Q/PLJ001-2011 method.
In such scheme, described ICA is buff powder, and density is about 1.12g/cm
3, fineness is that 150 μ m square hole sieves tail over 1.8%.
The above-mentioned early stage inhibition temperature rise later stage promotes the preparation method of the composite expanding agent of aquation, comprises the steps:
(1) by each constituent mass per-cent, take: calcium oxide 10～30%, sulphoaluminate cement clinker 28～43%, anhydrite 25～40%, magnesium oxide 5～15%, boric acid 0.3～0.5%, zinc sulfate 1～1.5%, ICA0.2～0.5%;
(2) calcium oxide, sulphoaluminate cement clinker and anhydrite are mixed, grinding is to specific surface area>=280m
2/ kg;
(3) by the magnesium oxide separate grinding to specific surface area>=450m
2/ kg; (4) by step 2) and the step 3) resulting materials is mixed with boric acid, zinc sulfate and ICA again, after homogenizing, obtain described composite expanding agent, and dress is sealed and deposited.
The mechanism of action of each component in composite expanding agent of the present invention: the present invention by reasonably combined light-burned calcium oxide, sulphoaluminate cement clinker, anhydrite volume and the magnesian volume of burning make that this composite expanded component is early stage in aquation, mid-term, later stage can react, produce and expand.In early expansion, sulfate ion, aluminum ion and calcium ion, alkaline media etc. generate ettringite, take ettringite as main expansion sources, ettringite combination and adsorbed 32 water moleculess, wherein dot matrix mortise water is 6,26 of coordinated water, this makes the solid volume of ettringite increase 125% left and right; Gypsum etc. generate the cement expansive material of calcium hydroxide with cement, water mix by hydration reaction, its expansion sources is Ca (OH)
2, after reaction, solid volume almost increases l doubly.Aluminium sulfate expanding agent and lime swelling agent are all just to produce a large amount of expansions in the length of time at 7d, MgO bang swollen dose owing to thering is the emblem of delay bulking effect, Main Function expanded in the middle and later periods, the direct drive energy of the expansion of the swelling agent of MgO is from Mg (OH)
2swelling power and the crystallization pressure of crystal, at the early stage Mg of aquation (OH)
2crystal is very tiny, and the expansion principal element of slurry is water suction swelling power, with Mg (OH)
2growing up of crystal, the crystalline growth pressure of crystal changes the major impetus of expansion into.Composite expanding agent of the present invention is introduced component I CA, at concrete mix initial stage savings large quantity of moisture, the part heat that the absorbent gelling material aquation produces, suppress the temperature rise of inside concrete aquation, and discharge in conjunction with water when interior humidity is unsaturated, improve the relative humidity of its surrounding environment, suppress on the one hand concrete self-constriction and dry shrinkage, promote on the other hand the especially continuation aquation of swelling agent of the gelling material such as cement, make concrete volumetric expansion and gain in strength cooperative development, guarantee the continual and steady expansion characteristics of later concrete.
In composite expanding agent, the mechanism of action of ICA is as follows: ICA has good wetting ability, sufficient water-retaining capacity; Good alkali capacitive and pressure-sensitive, take " high absorb water-stablize water storage-capable of realizing controlled-release water " be design objective, the employing tapioca (flour) is main chain, take unsaturated monoolefine as side chain, with amide group (CONH
2) and propanesulfonic acid group (SO
3h) be functional group, molecular structure as shown in the formula (I), belongs to tapioca (flour) polymer-modified.Free radical initiation, graft reaction, network cross-linked three phases are experienced in the formation of this polymer network structure graft copolymer altogether.In molecular structure, poly-hydroxy tapioca (flour) and high reactivity acrylamide and 2-acrylamide-2-methyl propane sulfonic monomer provide condition for Raolical polymerizable, hydrophilic and not too responsive amide group and sulfonic acid group provides guarantee for water storage stability to alkali, lightly crosslinked network structure provides space for holding enough moisture.
ICA in conjunction with being divided into Free water and fetter waetr in water, different on thermodynamic property and mechanical property, but bonding force is all more weak; Irreducible water is the moisture that is subject to intermolecular hydrogen bonding effect absorption, bonding force is slightly strong, be equivalent to the capillary water in concrete, its thermodynamic property and mechanical property are slightly different from the ortho-water in concrete, therefore the specific heat capacity of ICA is more concrete much larger, can be in the concrete hydrating exothermic process absorption portion heat, suppress the temperature rise of inside concrete aquation, improve the aquation process of gelling material.And the most water-cement ratio of modern concrete is low, use in a large number superfine active gelling material and high efficiency water reducing agent, structure height is closely knit, extraneous moisture can't enter inside concrete, inside concrete self-desiccation phenomenon is inevitable, causes hydration reaction limited, and swelling agent expands and can't continue to carry out.Decline along with inside concrete humidity, inevitably cause the inside concrete negative pressure to increase, when humidity and inside concrete capillary pressure reach certain value, ICA can be under unsaturated humidity environment original position the spontaneous water of releasing in time, supplemented the pore water consumption, eliminate the inside concrete self-desiccation, regulate internal medium humidity, guarantee the hydration swelling reaction continue carry out, reach abundant aquation, suppress to shrink, promoting to mix the concrete later stage of swelling agent continues to expand.In addition, by mixing boric acid and zinc sulfate, can delay the early stage speed of reaction of swelling agent aquation, weaken the peak height at hydration heat peak, postpone the time that exothermic peak occurs, with ICA, jointly bring into play the effect that reduces the aquation temperature rise, effectively improved the swelling agent phenomenon deteriorated to the concrete work performance.
Beneficial effect of the present invention: composite expanding agent prepared by (1) the present invention, its starting material wide material sources, economy is easy to get and Environmental compatibility good; (2) composite expanding agent of the present invention have advantages of early expansion can large, sustainable expansion and expansion stable period long, the energy concrete self-constriction of effective compensation and dry shrinkage, make concrete volumetric expansion and gain in strength cooperative development; (3) composite expanding agent of the present invention, can guarantee that steel pipe and core concrete form well " cuff " effect, also the problem that mass concrete is easy to occur temperature and shrinkage crack be can solve, concrete filled steel tube and mass concrete therefore are applicable to very much being applied to.
Embodiment
In order to understand better the present invention, further illustrate content of the present invention below in conjunction with embodiment and subordinate list, but content of the present invention not only is confined to following example.
Embodiment 1～5
A kind of early stage inhibition temperature rise later stage promotes the composite expanding agent of aquation, and its preparation process comprises the steps:
(1) take each component: calcium oxide, sulphoaluminate cement clinker, anhydrite, magnesium oxide, boric acid, zinc sulfate, and ICA, each constituent mass per-cent sees the following form 1; (2) calcium oxide, sulphoaluminate cement clinker and anhydrite are mixed, grinding is to specific surface area>=280m
2/ kg; (3) by the magnesium oxide separate grinding to specific surface area>=450m
2/ kg; (4) by step 2) and step 3) in resulting materials and step 1) remaining other material mixed, homogenizing, obtain described composite expanding agent, and dress is sealed and is deposited.
Described calcium oxide is light-burned calcium oxide, be by calcite after fragmentation, through 900～1100 ℃ of high-temperature calcinations, form;
Described sulphoaluminate cement clinker is by anhydrous calcium sulphoaluminate
tetracalcium aluminoferrite (C
4aF) and Dicalcium Phosphate (Feed Grade) (C
2s) form, the mass percent of each component is:
c
4aF:3.5～8%, C
2s:18.5～37.5%.
Described anhydrite is natural or artificial anhydrite;
Described magnesium oxide was burned magnesium oxide, was to be formed through 1300～1400 ℃ of high-temperature calcinations by magnesite its specific surface area>=450m
2/ kg, the measuring method of specific surface area is: " GB/T8074-2008 Method of determination for specific surface of cement (Bo Shi method) ";
Described boric acid is the white powder crystallization, and satiny feel is arranged, odorless, and density is about 1.43g/cm
3;
Described zinc sulfate is white powder, odorlessness, and puckery, density is about 1.96g/cm
3;
Described ICA is that tapioca (flour) is polymer-modified, and as shown in the formula (I), described ICA water-intake rate>=80g/g, release water rate>=80wt% to its structural formula, water-intake rate and release the water rate and measure with reference to the Q/PLJ001-2011 method; Described ICA is buff powder, and density is about 1.12g/cm
3, fineness is that 150 μ m square hole sieves tail over 1.8%.
In embodiment 1～3, described ICA prepares as follows:
(1) starch pasting: get the distilled water of 100ml, take the 2g tapioca (flour) and be dissolved in distilled water and stir, starch fluid is added in the four-hole bottle that agitator, reflux condensing tube and thermometer are housed, heating gelatinization;
(2) free radical causes: get the distilled water of 50ml, take the common 0.3g of ceric ammonium nitrate and ammonium persulphate and be dissolved in distilled water, wherein ceric ammonium nitrate: the mass ratio of ammonium persulphate is 1:9, after stirring, joins in the described four-hole boiling flask of step (1);
(3) graft copolymerization: get the distilled water of 100ml, take respectively the two Methacrylamides (linking agent) of 5g monomer acrylamide and 0.03g, water-soluble and stir, obtain monomer solution; Monomer solution need be added drop-wise in the described four-hole boiling flask of step (1) after the described radical initiation reaction 10min of step (2) again, controls monomer solution time for adding 1h under 60 ℃ of conditions;
(4) composite crosslinking: get in the distilled water that 2-acrylamide-2-methyl propane sulfonic (AMPS) is dissolved in 50ml and obtain AMPS solution, wherein the mass ratio of the described monomer acrylamide of 2-acrylamide-2-methyl propane sulfonic and step (3) is 1:6; Get a certain amount of water glass solution, with phenolphthalein, make developer, with water glass solution, drip AMPS solution, in AMPS solution, the color of phenolphthalein changes redness into gradually from colourless, and redness obtains pre-polysilicic acid sol azury while no longer taking off; The pre-polysilicic acid sol of gained is dropped in the described four-hole boiling flask of step (1), promote composite crosslinking by crossing powerful mechanical stirring (100r/min) effect, react 3h in 60 ℃ of environment, reaction obtains colourless spawn or contains the strong solution of colourless spawn after finishing;
(5) hydrolysis: get the distilled water of 100ml, NaOH is water-soluble, regulate pH value 12, join the described four-hole boiling flask of step (1), hydrolysis 30min obtains crude product;
(6) suction filtration, washing: with the vacuum filtration machine, crude product is dewatered, then with ethanol and acetone, crude product is soaked, washs, wash away residual alkali, monomer, at least carry out twice washing, obtain pure products;
(7) dry, grinding: pure products is dried to constant weight through vacuum drying oven, after fragmentation, grinding, obtains the ICA powder.
In embodiment 4, the preparation method of described ICA and embodiment 1～3 are roughly the same, and difference is: the tapioca (flour) quality that (1) takes is 1g; (2) ceric ammonium nitrate taken and the quality of ammonium persulphate are 0.1g; (3) quality of the monomer acrylamide taken is 0.1g, and the quality of two Methacrylamides is 0.01g, and the temperature of graft copolymerization is 50 ℃, and the time for adding of monomer solution is 0.5h; (4) mass ratio of 2-acrylamide-2-methyl propane sulfonic and monomer acrylamide is 1:1, and the mixing speed of composite crosslinking is 80r/min, and temperature of reaction is 50 ℃, and the reaction times is 2.5h; (5) hydrolysis: regulating the pH value is 10.
In embodiment 5, the preparation method of described ICA and embodiment 1～3 are roughly the same, and difference is: the tapioca (flour) quality that (1) takes is 4g; (2) ceric ammonium nitrate taken and the quality of ammonium persulphate are 0.5g; (3) quality of the monomer acrylamide taken is 10g, and the quality of two Methacrylamides is 0.05g, and the temperature of graft copolymerization is 80 ℃, and the time for adding of monomer solution is 0.7h; (4) mass ratio of 2-acrylamide-2-methyl propane sulfonic and monomer acrylamide is 1:9, and the mixing speed of composite crosslinking is 90r/min, and temperature of reaction is 80 ℃, and the reaction times is 2.5h; (5) hydrolysis: regulating the pH value is 11.
Each component percentages (%) of table 1 composite expanding agent
| Embodiment | Calcium oxide | Sulphoaluminate cement clinker | Anhydrite | MgO | Boric acid | Zinc sulfate | ICA |
| 1 | 10 | 43 | 35 | 10 | 0.3 | 1.5 | 0.2 |
| 2 | 15 | 38 | 40 | 5 | 0.4 | 1.3 | 0.3 |
| 3 | 18 | 36 | 36 | 8 | 0.4 | 1.2 | 0.4 |
| 4 | 24 | 30 | 32 | 12 | 0.5 | 1.1 | 0.4 |
| 5 | 30 | 28 | 25 | 15 | 0.5 | 1 | 0.5 |
The composite expanding agent that embodiment 1～5 is prepared is applied in concrete filled steel tube, performance is in Table 2, application result is in Table 3, the result of table 3 shows: this swelling agent can effectively improve concrete degree of free swelling for concrete filled steel tube, and also in continuation, improve to the concrete free expansion of 60d at 28d, illustrate that this swelling agent all can effectively improve concrete degree of free swelling at aquation initial stage and aquation later stage; Because this swelling agent causes the concrete early strength on the low side to the delayed action of aquation, the middle and later periods concrete continues to expand, concrete intensity fast lifting, finally reach effective concrete strength simultaneously, realizes the prolonged expansion of volume of concrete and the growth cooperative development of intensity.
The composite expanding agent that embodiment 1～5 is prepared is applied in mass concrete, performance is in Table 4, application result is in Table 5, the result of table 5 shows: this swelling agent can effectively improve concrete degree of free swelling for mass concrete, due to mass concrete under open environment, produce dry shrinkage, so remain unchanged or slightly reduce to the concrete free expansion of 60d at 28d, but the more blank sample of reduction value is much smaller, illustrate that this swelling agent still can effectively improve concrete degree of free swelling at aquation initial stage and aquation later stage, thereby the later stage that has reduced mass concrete shrinks.Simultaneously, this swelling agent causes the concrete early strength on the low side to the delayed action of aquation, along with concrete prolonged expansion of middle and later periods, and concrete intensity fast lifting, finally reach effective concrete strength, realize the prolonged expansion of volume of concrete and the growth cooperative development of intensity.
Performance (the kg/m of table 2 composite expanding agent in concrete filled steel tube
3)
Annotate: in the concrete mix stage, for making the ICA in swelling agent, fully absorb moisture, need to extend churning time, approximately 5～8min.
The application result of table 3 swelling agent in concrete filled steel tube
Annotate: the slump, divergence test are undertaken by GBT50080-2002; Intensity test is undertaken by GBT50081-2002; Degree of free swelling refers to the rate of expansion under the steel pipe air tight condition.
Performance (the kg/m of table 4 swelling agent in mass concrete
3)
Annotate: in the concrete mix stage, for making the ICA in swelling agent, fully absorb moisture, need to extend churning time, approximately 5～8min.
The application result of table 5 swelling agent in mass concrete
Annotate: the slump, divergence test are undertaken by GB/T50080-2002; Intensity test is undertaken by GB/T50081-2002; The degree of free swelling test is undertaken by GB/T50082-2009.
Obviously, above-described embodiment is only to be the example that clearly explanation is done, and is not the restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without also giving all embodiments.And the apparent variation of therefore amplifying or change are still within the protection domain in the invention.
Claims (10)
1. one kind is suppressed the composite expanding agent that the temperature rise later stage promotes aquation in early days, it is characterized in that it is comprised of calcium oxide, sulphoaluminate cement clinker, anhydrite, magnesium oxide, boric acid, zinc sulfate and ICA, the mass percent of each component is: calcium oxide 10～30%, sulphoaluminate cement clinker 28～43%, anhydrite 25～40%, magnesium oxide 5～15%, boric acid 0.3～0.5%, zinc sulfate 1～1.5%, ICA0.2～0.5%.
2. composite expanding agent according to claim 1, is characterized in that described calcium oxide is light-burned calcium oxide, be by calcite after fragmentation, through 900～1100 ℃ of high-temperature calcinations, form.
3. composite expanding agent according to claim 1, it is characterized in that, described sulphoaluminate cement clinker is comprised of anhydrous calcium sulphoaluminate, tetracalcium aluminoferrite and Dicalcium Phosphate (Feed Grade), the mass percent of each component is: anhydrous calcium sulphoaluminate: 55～75%, tetracalcium aluminoferrite: 3～8%, Dicalcium Phosphate (Feed Grade): 18.5～37.5%.
4. composite expanding agent according to claim 1, is characterized in that, described anhydrite is natural or artificial anhydrite.
5. composite expanding agent according to claim 1, is characterized in that, described magnesium oxide was burned magnesium oxide, was to be formed through 1300～1400 ℃ of high-temperature calcinations by magnesite its specific surface area>=450m
2/ kg.
6. composite expanding agent according to claim 1, is characterized in that, the fineness of described ICA is that 150 μ m square hole sieves tail over 1.8%.
7. composite expanding agent according to claim 1, is characterized in that, described ICA is that tapioca (flour) is polymer-modified, its structural formula as shown in the formula (I):
8. composite expanding agent according to claim 7, is characterized in that the preparation method of described ICA comprises the steps:
(1) starch pasting: take 1～4 portion of tapioca (flour) of weight part and be dissolved in distilled water and stir, then join in reactor, heating gelatinization;
(2) free radical causes: take ceric ammonium nitrate and ammonium persulphate totally 0.1～0.5 weight part be dissolved in distilled water, ceric ammonium nitrate wherein: the mass ratio of ammonium persulphate is 1:9, after stirring, joins in the described reactor of step (1);
(3) graft copolymerization: take respectively the two Methacrylamides of 0.1～10 weight parts monomers acrylamide and 0.01～0.05 weight part, water-soluble and stir, obtain monomer solution; Monomer solution need be added drop-wise in the described reactor of step (1) after the described radical initiation reaction 10min of step (2) again, and the time for adding of controlling monomer solution under 50～80 ℃ of conditions is 0.5～1h;
(4) composite crosslinking: get the 2-acrylamide-2-methyl propane sulfonic and be dissolved in distilled water and obtain 2-acrylamide-2-methyl propane sulfonic solution, wherein the mass ratio of the described monomer acrylamide of 2-acrylamide-2-methyl propane sulfonic and step (3) is 1:1～1:9; Get a certain amount of water glass solution, make developer with phenolphthalein, drip 2-acrylamide-2-methyl propane sulfonic solution with water glass solution, in 2-acrylamide-2-methyl propane sulfonic solution, the color of phenolphthalein is from the colourless redness that changes into gradually, and, when redness is no longer taken off, obtain pre-polysilicic acid sol azury; The pre-polysilicic acid sol of gained is dropped in the described reactor of step (1), the mechanical stirring rotating speed is 80～100r/min, temperature of reaction is 50～80 ℃, and the reaction times is 2.5～3h, and reaction obtains colourless spawn or contains the strong solution of colourless spawn after finishing;
(5) hydrolysis: NaOH is water-soluble, regulate pH value 10～12, join in the described reactor of step (1), hydrolysis obtains crude product;
(6) above-mentioned crude product, after suction filtration, is soaked with ethanol and acetone, and washing, obtain pure products;
(7) above-mentioned pure products is dried to constant weight, after broken and grinding, obtain the ICA powder.
9. composite expanding agent according to claim 7, is characterized in that water-intake rate >=80g/g of described ICA releases water rate >=80wt%.
10. described a kind of early stage inhibition temperature rise later stage of claim 1～9 promotes the preparation method of the composite expanding agent of aquation, it is characterized in that it comprises the steps:
(1) by each constituent mass per-cent, take: calcium oxide 10～30%, sulphoaluminate cement clinker 28～43%, anhydrite 25～40%, magnesium oxide 5～15%, boric acid 0.3～0.5%, zinc sulfate 1～1.5%, ICA0.2～0.5%;
(2) calcium oxide, sulphoaluminate cement clinker and anhydrite are mixed, grinding is to specific surface area>=280m
2/ kg;
(3) by the magnesium oxide separate grinding to specific surface area>=450m
2/ kg;
(4) above-mentioned steps (2) and step (3) resulting materials mixed with boric acid, zinc sulfate and ICA, after homogenizing, obtain described composite expanding agent, dress is sealed and is deposited.
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| CN105060793A (en) * | 2015-08-14 | 2015-11-18 | 武汉理工大学 | High titanium-bearing heavy slag C50 self-compacting weakly expansive concrete-filled steel tube and preparation method thereof |
| CN105084836A (en) * | 2015-08-14 | 2015-11-25 | 武汉理工大学 | C30 self-compaction microexpanded concrete-filled steel tube and preparation method thereof |
| CN106587831A (en) * | 2016-12-13 | 2017-04-26 | 武汉理工大学 | Super-elevation pumping marine concrete and preparation method thereof |
| CN106904911A (en) * | 2017-03-16 | 2017-06-30 | 海南瑞泽新型建材股份有限公司 | A kind of anti-corrosion maritime concrete of sea sand and preparation method thereof |
| CN107540258A (en) * | 2017-10-25 | 2018-01-05 | 桐城市永锦建筑工程有限公司 | A kind of concrete anticracking swelling agent |
| CN107827389A (en) * | 2017-11-07 | 2018-03-23 | 常州福隆工控设备有限公司 | A kind of preparation method of continual and steady intumescent swelling agent |
| CN107935504A (en) * | 2017-11-27 | 2018-04-20 | 江西省萍乡市联友建材有限公司 | Early strengthening and high strengthening, microdilatancy, the bar connecting sleeve grouting material of since conservation function |
| CN108503250A (en) * | 2018-03-07 | 2018-09-07 | 湖北乾道新型材料有限责任公司 | Cement expansive material and preparation method |
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| CN104386938A (en) * | 2014-10-30 | 2015-03-04 | 中冶天工集团有限公司 | Multifunctional expanding agent for seamless construction of super-long concrete structure |
| CN104496261A (en) * | 2014-11-21 | 2015-04-08 | 于芳 | Expansion rate and concrete strength development coordinated concrete expansive agent |
| CN104909596A (en) * | 2015-04-03 | 2015-09-16 | 中国建筑股份有限公司 | High efficiency composite expanding agent for high-strength self-stressing concrete filled steel tube and preparation method thereof |
| CN104788034A (en) * | 2015-04-17 | 2015-07-22 | 武汉工程大学 | Preparation method of phosphogypsum based high-energy long-acting expanding agent |
| CN105084836B (en) * | 2015-08-14 | 2017-08-25 | 武汉理工大学 | A kind of C30 self-compacting micro-expanded steel tube concretes and preparation method thereof |
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| CN107540258A (en) * | 2017-10-25 | 2018-01-05 | 桐城市永锦建筑工程有限公司 | A kind of concrete anticracking swelling agent |
| CN107827389A (en) * | 2017-11-07 | 2018-03-23 | 常州福隆工控设备有限公司 | A kind of preparation method of continual and steady intumescent swelling agent |
| CN107935504A (en) * | 2017-11-27 | 2018-04-20 | 江西省萍乡市联友建材有限公司 | Early strengthening and high strengthening, microdilatancy, the bar connecting sleeve grouting material of since conservation function |
| CN108585572A (en) * | 2018-02-05 | 2018-09-28 | 武汉优城科技有限公司 | A kind of polymer surface modification sulphoaluminate expander and preparation method thereof |
| CN108503250A (en) * | 2018-03-07 | 2018-09-07 | 湖北乾道新型材料有限责任公司 | Cement expansive material and preparation method |
| CN109231866A (en) * | 2018-10-12 | 2019-01-18 | 天津市金盛源特种建材有限公司 | A kind of heat of hydration suppressive cement expansive material and preparation method thereof |
| CN109231866B (en) * | 2018-10-12 | 2021-10-22 | 天津市金盛源特种建材有限公司 | Hydration heat inhibition type concrete expanding agent and preparation method thereof |
| CN112094630A (en) * | 2020-11-17 | 2020-12-18 | 东营东方化学工业有限公司 | Composite component resin cross-linking agent and preparation method thereof |
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