CN103435317B - 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 suppression temperature rise later stage promotion aquation and preparation method thereof.
Background technology
Because modern material prepares the continuous progress of level and building construction technology, the construction of the steel pipe arch bridge of super high rise building and Long span is more and more subject to people's favor, and therefore the engineer applied of concrete filled steel tube and mass concrete is very frequent.But current steel tube concrete soil material, common intensity grade is high, and gel material content is large, and water-cement ratio is low, and be in steel pipe airtight, cannot 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 greatly limited, be difficult to continual and steady expansion, be easy to the phenomenon causing concrete and steel pipe " to come to nothing ", make the globality of structure impaired, affect its bearing capacity and work-ing life greatly; And the heat of hydrated cementitious not easily sheds in mass concrete, aquation temperature rise is large, makes the table temperature difference in concrete large, is easy to cause uneven temperature deformation and thermal stress, causes the generation of thermal cracking thus, affect its weather resistance.Although mix swelling agent to compensate its self-constriction and dry shrinkage in mass concrete, 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 long, aquation temperature rise can be suppressed, and the later stage spontaneously can release water, regulate ambient humidity, ensure 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
A kind of early stage suppression temperature rise later stage is the object of the present invention is to provide 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 composite expanding agent of early stage suppression temperature rise later stage promotion aquation, be made up 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%.
In such scheme, described calcium oxide is light-burned calcium oxide, is by calcite after fragmentation, forms through 900 ~ 1100 DEG C of high-temperature calcinations.
In such scheme, described sulphoaluminate cement clinker is by anhydrous calcium sulphoaluminate
tetracalcium aluminoferrite (C
4and Dicalcium Phosphate (Feed Grade) (C AF)
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 DEG C 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 white powder crystallization, and have satiny feel, odorless, 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 weight part 1 ~ 4 portion of tapioca (flour) and be dissolved in distilled water and stir, then join in reactor, heating also gelatinization;
(2) free radical causes: take ceric ammonium nitrate and ammonium persulphate totally 0.1 ~ 0.5 weight part be dissolved in distilled water, wherein ceric ammonium nitrate: the mass ratio of ammonium persulphate is 1:9, joins in the reactor described in step (1) after stirring;
(3) graft copolymerization: take the two Methacrylamide of 0.1 ~ 10 weight parts monomers acrylamide and 0.01 ~ 0.05 weight part respectively, water-soluble and stir, obtain monomer solution; Monomer solution need be added drop-wise in step (1) described reactor after step (2) described radical initiation reaction 10min again, and the time for adding controlling monomer solution under 50 ~ 80 DEG C of conditions is 0.5 ~ 1h;
(4) composite crosslinking: get 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 2-acrylamide-2-methyl propane sulfonic and step (3) described monomeric acrylamide is 1:1 ~ 1:9; Get a certain amount of water glass solution, developer is made with phenolphthalein, 2-acrylamide-2-methyl propane sulfonic solution is dripped with water glass solution, when in 2-acrylamide-2-methyl propane sulfonic solution, the color of phenolphthalein changes redness into gradually from colourless, and when redness is no longer taken off, obtain pre-polysilicic acid sol azury; Pre-for gained polysilicic acid sol is dropped in step (1) described reactor, mechanical stirring rotating speed is 80 ~ 100r/min, temperature of reaction is 50 ~ 80 DEG C, and the reaction times is 2.5 ~ 3h, obtains colorless gel shape material or the strong solution containing colorless gel shape material after reaction terminates;
(5) be hydrolyzed: NaOH is water-soluble, and adjust ph 10 ~ 12, joins in step (1) described reactor, hydrolysis obtains crude product;
(6) above-mentioned crude product is after suction filtration, soaks with ethanol and acetone, and washing, obtains pure products;
(7) above-mentioned pure products is dried to constant weight, after fragmentation and grinding, obtain ICA powder.
In such scheme, the water-intake rate >=80g/g of described ICA, releases water rate >=80wt%, water-intake rate and release water rate and measure with reference to Q/PLJ001-2011 method.
In such scheme, described ICA is buff powder, and density is about 1.12g/cm
3, fineness is that 150 μm of square hole sieves tail over 1.8%.
The preparation method of the composite expanding agent of above-mentioned early stage suppression temperature rise later stage promotion aquation, comprises the steps:
(1) take by each constituent mass per-cent: 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 magnesium oxide separate grinding to specific surface area>=450m
2/ kg; (4) by step 2) and step 3) resulting materials carries out with boric acid, zinc sulfate and ICA mixing again, after homogenizing, obtain described composite expanding agent, and fill encapsulating and deposit.
The mechanism of action of each component in composite expanding agent of the present invention: by reasonably combined light-burned calcium oxide, sulphoaluminate cement clinker, anhydrite volume and the magnesian volume of burning, the present invention makes that this composite expanded component is early stage in aquation, mid-term, later stage can react, and produces and expands.In early expansion, sulfate ion, aluminum ion and calcium ion, alkaline media etc. generate ettringite, take ettringite as main expansion source, ettringite combines and has adsorbed 32 water moleculess, wherein 6, dot matrix mortise water, coordinated water 26, this makes the solid volume of ettringite increase about 125%; Generate the cement expansive material of calcium hydroxide after gypsum etc. and cement, water mix through 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 produce a large amount of expansions within 7d length of time, MgO bang swollen dose postpone emblem bulking effect owing to having, mainly acting on the middle and later periods expands, and the expansion Direct driver of the swelling agent of MgO can be derived from Mg (OH)
2the swelling power of crystal and crystallization pressure, 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 introduces component I CA, at concrete mix initial stage savings large quantity of moisture, the partial heat that absorbent gelling material aquation produces, suppress the temperature rise of inside concrete aquation, and discharge Bound moisture when interior humidity is unsaturated, improve the relative humidity of its surrounding environment, suppress concrete self-constriction and dry shrinkage on the one hand, promote on the other hand the continuation aquation of the gelling material such as cement especially swelling agent, make concrete volumetric expansion and gain in strength cooperative development, ensure 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, with " height absorb water-stablizes water storage-realizing controlled-release water ", for design objective, employing tapioca (flour) is main chain, with unsaturated monoolefine for 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 are that Raolical polymerizable provides condition, hydrophilic and be that water storage stability provides guarantee to the not too responsive amide group of alkali and sulfonic acid group, lightly crosslinked network structure provides space for holding enough moisture.
Free water and fetter waetr is divided in the Bound moisture of ICA, different in thermodynamic property and mechanical property, but bonding force is all more weak; Irreducible water is the moisture by intermolecular hydrogen bonding effect absorption, bonding force is slightly strong, be equivalent to the capillary water in concrete, its thermodynamic property is slightly different from the ortho-water in concrete with mechanical property, therefore the specific heat capacity of ICA is more concrete much larger, can in concrete hydrating exothermic process absorption portion heat, suppress the temperature rise of inside concrete aquation, improve the heat evolution velocity of gelling material.And the most water-cement ratio of modern concrete low, a large amount of use superfine active gelling material and high efficiency water reducing agent, structure height are closely knit, outside moisture cannot enter inside concrete, inside concrete self-desiccation phenomenon is inevitable, causes hydration reaction limited, and swelling agent expands and cannot continue to carry out.Along with the decline of inside concrete humidity, inside concrete negative pressure is inevitably caused to increase, when humidity and inside concrete capillary pressure reach certain value, ICA can under unsaturated humidity environment original position spontaneously in time release water, supplement pore water consumption, eliminate inside concrete self-desiccation, regulate internal medium humidity, what guarantee hydration swelling reacted continues to carry out, and reaches abundant aquation, suppresses to shrink, and promotes to mix the continuation expansion of swelling agent concrete later stage.In addition, by mixing boric acid and zinc sulfate, the speed of reaction that swelling agent aquation is early stage can be delayed, weaken the peak height at hydration heat peak, postpone the time that exothermic peak occurs, jointly play with ICA the effect reducing aquation temperature rise, effectively improve the phenomenon of swelling agent to the deterioration of concrete work performance.
Beneficial effect of the present invention: composite expanding agent prepared by (1) the present invention, its raw material sources is extensively, economy is easy to get and Environmental compatibility is good; (2) composite expanding agent of the present invention has the advantage of early expansion large, the sustainable expansion of energy and expansion stable period length, and 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 can solve the problem that mass concrete is easy to occur temperature and shrinkage crack, therefore be applicable to very much being applied to concrete filled steel tube and mass concrete.
Embodiment
In order to understand the present invention better, illustrate content of the present invention further below in conjunction with embodiment and subordinate list, but content of the present invention is not only confined to example below.
Embodiment 1 ~ 5
A composite expanding agent for early stage suppression temperature rise later stage promotion aquation, its preparation process comprises the steps:
(1) each component is taken: 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 magnesium oxide separate grinding to specific surface area>=450m
2/ kg; (4) by step 2) and step 3) in resulting materials and step 1) other material remaining carry out mixing, homogenizing, obtain described composite expanding agent, and fill encapsulating and deposit.
Described calcium oxide is light-burned calcium oxide, is by calcite after fragmentation, forms through 900 ~ 1100 DEG C of high-temperature calcinations;
Described sulphoaluminate cement clinker is by anhydrous calcium sulphoaluminate
tetracalcium aluminoferrite (C
4and Dicalcium Phosphate (Feed Grade) (C AF)
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 DEG C 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 white powder crystallization, and have satiny feel, odorless, 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, releases water rate>=80wt% to its structural formula, water-intake rate and release water rate and measure with reference to Q/PLJ001-2011 method; Described ICA is buff powder, and density is about 1.12g/cm
3, fineness is that 150 μm of square hole sieves tail over 1.8%.
In embodiment 1 ~ 3, described ICA prepares as follows:
(1) starch pasting: the distilled water getting 100ml, takes 2g tapioca (flour) and is dissolved in distilled water and stirs, and is added by starch fluid in the four-hole bottle that agitator, reflux condensing tube and thermometer are housed, heating also gelatinization;
(2) free radical causes: the distilled water getting 50ml, take ceric ammonium nitrate and ammonium persulphate altogether 0.3g be dissolved in distilled water, wherein ceric ammonium nitrate: the mass ratio of ammonium persulphate is 1:9, joins in the four-hole boiling flask described in step (1) after stirring;
(3) graft copolymerization: the distilled water getting 100ml, takes the two Methacrylamide (linking agent) of 5g monomeric acrylamide and 0.03g respectively, water-soluble and stir, and obtains monomer solution; Monomer solution need be added drop-wise in step (1) described four-hole boiling flask after step (2) described radical initiation reaction 10min again, controls monomer solution time for adding 1h under 60 DEG C of conditions;
(4) composite crosslinking: get 2-acrylamide-2-methyl propane sulfonic (AMPS) and be dissolved in the distilled water of 50ml and obtain AMPS solution, wherein the mass ratio of 2-acrylamide-2-methyl propane sulfonic and step (3) described monomeric acrylamide is 1:6; Get a certain amount of water glass solution, make developer with phenolphthalein, drip AMPS solution with water glass solution, when in AMPS solution, the color of phenolphthalein changes redness into gradually from colourless, and when redness is no longer taken off, obtain pre-polysilicic acid sol azury; Pre-for gained polysilicic acid sol is dropped in step (1) described four-hole boiling flask, composite crosslinking is promoted by crossing powerful mechanical stirring (100r/min) effect, in 60 DEG C of environment, react 3h, after reaction terminates, obtain colorless gel shape material or the strong solution containing colorless gel shape material;
(5) be hydrolyzed: the distilled water getting 100ml, NaOH is water-soluble, and regulate pH value 12, join step (1) described four-hole boiling flask, hydrolysis 30min obtains crude product;
(6) suction filtration, washing: dewater to crude product with vacuum filtration machine, then soaks crude product with ethanol and acetone, 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 ICA powder.
In embodiment 4, the preparation method of described ICA is roughly the same with embodiment 1 ~ 3, 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 monomeric acrylamide taken is 0.1g, and the quality of two Methacrylamide is 0.01g, and the temperature of graft copolymerization is 50 DEG C, and the time for adding of monomer solution is 0.5h; (4) mass ratio of 2-acrylamide-2-methyl propane sulfonic and monomeric acrylamide is 1:1, and the mixing speed of composite crosslinking is 80r/min, and temperature of reaction is 50 DEG C, and the reaction times is 2.5h; (5) be hydrolyzed: adjust ph is 10.
In embodiment 5, the preparation method of described ICA is roughly the same with embodiment 1 ~ 3, 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 monomeric acrylamide taken is 10g, and the quality of two Methacrylamide is 0.05g, and the temperature of graft copolymerization is 80 DEG C, and the time for adding of monomer solution is 0.7h; (4) mass ratio of 2-acrylamide-2-methyl propane sulfonic and monomeric acrylamide is 1:9, and the mixing speed of composite crosslinking is 90r/min, and temperature of reaction is 80 DEG C, and the reaction times is 2.5h; (5) be hydrolyzed: adjust ph 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 prepares 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 is used for can effectively improving concrete degree of free swelling in concrete filled steel tube, and also improve in continuation in the concrete free expansion of 28d to 60d, illustrate that this swelling agent all can effectively improve concrete degree of free swelling at aquation initial stage and aquation later stage; Because the delayed action of this swelling agent to aquation causes concrete early strength on the low side, middle and later periods concrete continues to expand, concrete intensity fast lifting, finally reaches effective concrete strength, realizes the prolonged expansion of volume of concrete and the growth cooperative development of intensity simultaneously.
The composite expanding agent that embodiment 1 ~ 5 prepares 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 is used for can effectively improving concrete degree of free swelling in mass concrete, under mass concrete is in open environment, produce dry shrinkage, so remain unchanged in the concrete free expansion of 28d to 60d or slightly reduce, but the more blank sample of decreasing 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, thus decrease the later stage contraction of mass concrete.Simultaneously, the delayed action of this swelling agent to aquation causes concrete early strength on the low side, along with middle and later periods concrete prolonged expansion, 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)
Note: in the concrete mix stage, for making the ICA in swelling agent fully absorb moisture, need extend churning time, about 5 ~ 8min.
The application result of table 3 swelling agent in concrete filled steel tube
Note: the test of the slump, divergence is undertaken by GBT50080-2002; Intensity test is undertaken by GBT50081-2002; Degree of free swelling refers to the rate of expansion under steel pipe air tight condition.
Performance (the kg/m of table 4 swelling agent in mass concrete
3)
Note: in the concrete mix stage, for making the ICA in swelling agent fully absorb moisture, need extend churning time, about 5 ~ 8min.
The application result of table 5 swelling agent in mass concrete
Note: the test of the slump, divergence is undertaken by GB/T50080-2002; Intensity test is undertaken by GB/T50081-2002; Degree of free swelling test is undertaken by GB/T50082-2009.
Obviously, above-described embodiment is only for the example done clearly is described, and the restriction not 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 the need to also giving all embodiments.And therefore amplified apparent change or variation are still within the protection domain of the invention.
Claims (6)
1. one kind is suppressed the temperature rise later stage to promote the composite expanding agent of aquation in early days, it is characterized in that it is made up 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%, ICA 0.2 ~ 0.5%;
Described calcium oxide is light-burned calcium oxide, is by calcite after fragmentation, forms through 900 ~ 1100 DEG C of high-temperature calcinations; Described sulphoaluminate cement clinker is made up of anhydrous calcium sulphoaluminate, tetracalcium aluminoferrite and Dicalcium Phosphate (Feed Grade), and the mass percent of each component is: anhydrous calcium sulphoaluminate: 55 ~ 75%, tetracalcium aluminoferrite: 3 ~ 8%, Dicalcium Phosphate (Feed Grade): 18.5 ~ 37.5%; Described magnesium oxide was burned magnesium oxide, was to be formed through 1300 ~ 1400 DEG C of high-temperature calcinations by magnesite, its specific surface area>=450m
2/ kg; Described ICA is that tapioca (flour) is polymer-modified, and its structural formula is such as formula shown in (I):
2. composite expanding agent according to claim 1, it is characterized in that, described anhydrite is natural or artificial anhydrite.
3. composite expanding agent according to claim 1, it is characterized in that, the fineness of described ICA is that 150 μm of square hole sieves tail over 1.8%.
4. composite expanding agent according to claim 1, is characterized in that the preparation method of described ICA comprises the steps:
(1) starch pasting: take weight part 1 ~ 4 portion of tapioca (flour) and be dissolved in distilled water and stir, then join in reactor, heating also gelatinization;
(2) free radical causes: take ceric ammonium nitrate and ammonium persulphate totally 0.1 ~ 0.5 weight part be dissolved in distilled water, wherein ceric ammonium nitrate: the mass ratio of ammonium persulphate is 1:9, joins in the reactor described in step (1) after stirring;
(3) graft copolymerization: take the two Methacrylamide of 0.1 ~ 10 weight parts monomers acrylamide and 0.01 ~ 0.05 weight part respectively, water-soluble and stir, obtain monomer solution; Monomer solution need be added drop-wise in step (1) described reactor after step (2) described radical initiation reaction 10min again, and the time for adding controlling monomer solution under 50 ~ 80 DEG C of conditions is 0.5 ~ 1h;
(4) composite crosslinking: get 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 2-acrylamide-2-methyl propane sulfonic and step (3) described monomeric acrylamide is 1:1 ~ 1:9; Get a certain amount of water glass solution, developer is made with phenolphthalein, 2-acrylamide-2-methyl propane sulfonic solution is dripped with water glass solution, when in 2-acrylamide-2-methyl propane sulfonic solution, the color of phenolphthalein changes redness into gradually from colourless, and when redness is no longer taken off, obtain pre-polysilicic acid sol azury; Pre-for gained polysilicic acid sol is dropped in step (1) described reactor, mechanical stirring rotating speed is 80 ~ 100r/min, temperature of reaction is 50 ~ 80 DEG C, and the reaction times is 2.5 ~ 3h, obtains colorless gel shape material or the strong solution containing colorless gel shape material after reaction terminates;
(5) be hydrolyzed: NaOH is water-soluble, and adjust ph 10 ~ 12, joins in step (1) described reactor, hydrolysis obtains crude product;
(6) above-mentioned crude product is after suction filtration, soaks with ethanol and acetone, and washing, obtains pure products;
(7) above-mentioned pure products is dried to constant weight, after fragmentation and grinding, obtain ICA powder.
5. composite expanding agent according to claim 1, is characterized in that the water-intake rate >=80g/g of described ICA releases water rate >=80wt%.
6. in Claims 1 to 5, arbitrary described a kind of early stage suppression temperature rise later stage promotes the preparation method of the composite expanding agent of aquation, it is characterized in that it comprises the steps:
(1) take by each constituent mass per-cent: 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%, ICA 0.2 ~ 0.5%;
(2) calcium oxide, sulphoaluminate cement clinker and anhydrite are mixed, grinding is to specific surface area>=280m
2/ kg;
(3) by magnesium oxide separate grinding to specific surface area>=450m
2/ kg;
(4) above-mentioned steps (2) and step (3) resulting materials are carried out with boric acid, zinc sulfate and ICA mix, after homogenizing, obtain described composite expanding agent, dress encapsulating is deposited.
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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 |
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 |
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 |
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 |
CN112094630B (en) * | 2020-11-17 | 2021-05-28 | 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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CN1317219C (en) * | 2005-09-22 | 2007-05-23 | 武汉理工大学 | Method of controlling expansion of steel pipe concrete precisely |
CN1314617C (en) * | 2005-09-22 | 2007-05-09 | 武汉理工大学 | High-energy delay expanding agent for closed concrete and its prepn |
CN1300039C (en) * | 2005-09-22 | 2007-02-14 | 武汉理工大学 | Expansion designable high strength steel pipe concrete and its prepn |
CN102351501A (en) * | 2011-07-04 | 2012-02-15 | 武汉理工大学 | Cement-based grouting material and preparation method thereof |
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