CN104692688B - A kind of modified oxidized calcium class cement concrete swelling agent and preparation method thereof - Google Patents
A kind of modified oxidized calcium class cement concrete swelling agent and preparation method thereof Download PDFInfo
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- CN104692688B CN104692688B CN201510060121.XA CN201510060121A CN104692688B CN 104692688 B CN104692688 B CN 104692688B CN 201510060121 A CN201510060121 A CN 201510060121A CN 104692688 B CN104692688 B CN 104692688B
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- swelling agent
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- calcium oxide
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Abstract
The present invention provides a kind of modified oxidized calcium class cement concrete swelling agent and preparation method thereof.The specific surface area of the modified oxidized calcium class cement concrete swelling agent is 100 600 m2/ kg, is made up of, water soluble polymer organic polymer is wrapped in the surface of calcium oxide expansive clinker water soluble polymer organic polymer and calcium oxide expansive clinker, accounts for 1% the 20% of the modified oxidized calcium class cement concrete swelling agent quality total amount.The cement concrete swelling agent of the present invention can reduce the invalid aquation of concrete plastic stage, and the swell increment after increase hardening, available for the anti-crack and anti-seepage of concrete structure, increases substantially the durability of concrete structure.
Description
Technical field
The invention belongs to construction material technical field of concrete additives, more particularly to a kind of modified oxidized calcium cement is mixed
Solidifying soil expansion agent and preparation method thereof.
Background technology
Cement concrete is most large construction material in the world at present, cheap, is widely used.But coagulating cement
Native easily shrinkage cracking, crack can make the reinforcing bar in concrete occur corrosion, shorten the service life of engineering structure, have a strong impact on
The durability of concrete.
The problem of in order to solve cement concrete easy shrinkage cracking, researcher has invented expanding cement and cement concrete
Swelling agent.Since 1930s French invention expanding cement, particularly from Japan on the basis of expanding cement by it
In expansion component be isolated as the swelling agent that individually fills since, cement expansive material gradually develops into Concrete Industry
One of maximum additive of middle consumption, is widely used in underground waterproof seepage control project, super-long structural and all kinds of large-scale coagulations
Native construction work, as preventing the effective technology of Shrinkage Cracking of Concrete.
Calcium oxide expansive clinker is one kind of cement concrete swelling agent, and domestic research is relatively fewer, a reason
It is the easy moisture absorption of expansive clinker and fails, clinker storage period is short；Another is more main reasons is that calcium oxide expansive clinker and water
It is swift in response, most of expansion energy consumption makees idle work in concrete plastic stage.
Therefore need to be improved raising to calcium oxide expansive clinker.How calcium oxide expansive clinker and water are delayed
Contact, reduces the consumption of cement concrete plastic stage expansive clinker, and effective expansion energy after increase concrete hardening is oxidation
One of difficult point of the research of calcium class expansive clinker and performance boost.
Publication number CN103130437A Chinese patent literature discloses a kind of preparation method of cement expansive material, is to use
Gypsum and calcium oxide melting calcining is formed gypsum wrap up calcium oxide expansive clinker, further with other powder intergrindings to than
Surface area 140-400m2Obtained after/kg.The swelling agent weatherability of the invention has strengthened, and shelf life of products there has also been
Extension, but the problem of concrete plastic stage swelling agent is consumed excessively can not be solved.
The content of the invention
It is swift in response for calcium oxide expansive clinker and water, the expansion energy of calcium oxide expansive clinker is in concrete plasticity
The problem of discrete consuming is excessive, the present invention provides a kind of modified oxidized calcium class cement concrete swelling agent and preparation method thereof, subtracts
Its few expansion energy after the invalid expansion, increase concrete hardening of concrete plastic stage.
Modified oxidized calcium class cement concrete swelling agent of the present invention is to utilize water soluble polymer organic polymer pair
Calcium oxide surface carry out parcel modification, calcium oxide expansive clinker surface formed diaphragm, as transition zone, delay its with
The time of contact of water, the reaction of concrete plastic stage calcium oxide and water is reduced, reduce swelling agent in concrete plastic stage
Invalid expansion.Simultaneously as macromolecule organic polymer has water solubility, moisture is on the one hand delayed to enter inside calcium oxide particle
The speed reacted, on the other hand provides required after the water-soluble polymer water suction on calcium oxide surface for the aquation of calcium oxide
Moisture；So as to reach the purpose for improving calcium oxide expansive clinker expansion character.
Modified oxidized calcium class cement concrete swelling agent of the present invention, by water soluble polymer organic polymer and oxidation
Calcium class expansive clinker is constituted, and the water soluble polymer organic polymer is wrapped in the surface of calcium oxide expansive clinker；It is described
Water soluble polymer organic polymer accounts for the 1%-20% of the modified oxidized calcium class cement concrete swelling agent quality total amount, institute
The specific surface area for stating modified oxidized calcium class cement concrete swelling agent is 100-600m2/kg。
The number-average molecular weight of the water soluble polymer organic polymer is 1-500kg/mol；Selected from polyacrylamide, gather
The mixing of one kind and any of the above ratio in methacrylic acid, polyacrylic acid, PVP, PEO
Thing.
The calcium oxide expansion agents clinker can be commercially available, and its specific surface area is 100-600m2/ kg, wherein free oxidation
Calcium content (f-CaO) >=60%.
The calcium oxide expansive clinker can also by lime stone and composite mineralizer combined grinding into after raw material in 1200-
Calcine grinding at 1500 DEG C to form, its specific surface area is 100-600m2/kg；
Wherein the mass ratio of composite mineralizer and lime stone is 0：100~10：90；
Composite mineralizer by mass percentage content be 40%-100% gypsum, 0%-60% aluminum oxide and/or sulphur
Sour aluminium composition.
The preparation method of modified oxidized calcium class cement concrete swelling agent of the present invention, comprises the steps：
A) by lime stone and composite mineralizer combined grinding into the calcining at 1200-1500 DEG C after raw material, grinding is to than table
Area is 100-600m2/ kg, obtains calcium oxide expansive clinker；
B) macromolecule organic polymer is dissolved with anhydrous organic solvent, adds the calcium oxide expansive clinker mixing of metering
Uniformly, residual organic solvents are removed, grinding to specific surface area is 100-600m2/kg；
The anhydrous organic solvent is in dry dichloromethane, chloroform, tetrahydrofuran, acetone, toluene, dimethylbenzene
More than one arbitrary proportion mixtures.
The application process of modified oxidized calcium class cement concrete swelling agent of the present invention：In production, mixed concrete
When, modified oxidized calcium class cement concrete swelling agent of the present invention is together added with other binder materials can produce receipts
Contracting compensating action；Or as needed by the same gypsum of modified oxidized calcium class cement concrete swelling agent of the present invention, flyash etc.
After material is with certain mass ratio mixing, then together with gelling system mix is added, can equally produce shrinkage-compensating effect.This
The consumption of the described modified oxidized calcium class cement concrete swelling agent of invention is the 0-10% of total gel rubber material consumption.
Compared with prior art products, modified oxidized calcium class cement concrete swelling agent of the present invention reduces plasticity rank
Section swelling agent aquation, increases hardening phase expansion energy, can further reduce or remit concrete structure because of early-age shrinkage, drying shrinkage and shrinkage
Harmful cracks are produced, structural leakage problem is overcome, available for the anti-crack and anti-seepage of general concrete structure, and can increase substantially mixed
Coagulate the durability of soil.
Brief description of the drawings
Fig. 1：The stereoscan photograph of modified oxidized calcium class cement concrete swelling agent 1 prepared by embodiment 1
Fig. 2：The modified oxidized calcium class cement concrete swelling agent 1 and the unmodified calcium oxide of contrast of the gained of embodiment 1
The micro Thermal test result of expansive clinker 1 '
Fig. 3-8：Modified oxidized calcium class cement concrete swelling agent in embodiment 1-6 and accordingly contrast unmodified oxidation
Contraction result of the calcium class expansive clinker in cement paste system
Specific embodiment
According to following embodiments, the present invention may be better understood.However, as it will be easily appreciated by one skilled in the art that real
Apply specific material proportion, process conditions and its result described by example and be merely to illustrate the present invention, without that will not also should limit
The present invention described in detail in claims processed.Wherein, polymer is bought from Aladdin Reagent Company and SIGMA-
ALDRICH Reagent Companies.
Embodiment 1
It is 90 by mass ratio：It is through ball mill intergrinding to fineness after 10 lime stone and composite mineralizer mixing
200m2/ kg raw meal powder, wherein composite mineralizer are gypsum.Raw meal powder after grinding is calcined at 1200 DEG C, and in the temperature
The lower insulation 120min of degree (calcination time at i.e. 1200 DEG C is 120min), insulation takes out firing sample in air immediately after terminating
Middle quenching, grinding to fineness is 200m2Calcium oxide expansive clinker is made in/kg.
Obtained calcium oxide expansive clinker is added into number-average molecular weight molten for the dichloromethane of 5kg/mol polyethylene glycol
In liquid, calcium oxide and PEG4KMass ratio be 99:Remove methylene chloride after 1, stirring 5min, gained solid through grinding to than
Surface area is 500m2/ kg, packs and obtains modified oxidized calcium class cement concrete swelling agent 1 of the present invention.
As a comparison, the calcium oxide expansive clinker of above-mentioned long time without surface modification is labeled as 1 '.
Embodiment 2
It is 99 by mass ratio：It is through ball mill intergrinding to fineness after 1 lime stone and composite mineralizer mixing
100m2/ kg raw meal powder, wherein composite mineralizer are that mass ratio is 50:25:25 gypsum/aluminum oxide/aluminum sulfate.By grinding
Raw meal powder afterwards is calcined at 1350 DEG C, and is incubated 60min at such a temperature, and insulation takes out firing sample in sky immediately after terminating
Quenching in gas, grinding to fineness is 100m2Calcium oxide expansive clinker is made in/kg.
Obtained calcium oxide expansive clinker is added into three chloromethanes of the number-average molecular weight for 10kg/mol polyacrylamide
In alkane solution, the mass ratio of calcium oxide and polyacrylamide is 80:Solvent chloroform is removed after 20, stirring 5min, gained is solid
Body is 600m through grinding to specific surface area2/ kg, packs that to obtain modified oxidized calcium class cement concrete of the present invention swollen
Swollen dose 2.
As a comparison, the calcium oxide expansive clinker of above-mentioned long time without surface modification is labeled as 2 '.
Embodiment 3
It is 95 by mass ratio：It is through ball mill intergrinding to fineness after 5 lime stone and composite mineralizer mixing
600m2/ kg raw meal powder, wherein composite mineralizer are that mass ratio is 30:50:20 gypsum/aluminum sulfate/aluminum oxide.By grinding
Raw meal powder afterwards is calcined at 1450 DEG C, and is incubated 40min at such a temperature, and insulation takes out firing sample in sky immediately after terminating
Quenching in gas, grinding to fineness is 600m2Calcium oxide expansive clinker is made in/kg.
Obtained calcium oxide expansive clinker is added into tetrahydrochysene of the number-average molecular weight for 50kg/mol polymethylacrylic acid
In tetrahydrofuran solution, the mass ratio of calcium oxide and polymethylacrylic acid is 90:Solvents tetrahydrofurane is removed after 10, stirring 15min, institute
It is 450m that solid, which is obtained, through grinding to specific surface area2/ kg, packs and obtains modified oxidized calcium class coagulating cement of the present invention
Soil expansion agent 3.
As a comparison, the calcium oxide expansive clinker of above-mentioned long time without surface modification is labeled as 3 '.
Embodiment 4
It is 98 by mass ratio：It is through ball mill intergrinding to fineness after 2 lime stone and composite mineralizer mixing
360m2/ kg raw meal powder, wherein composite mineralizer are that mass ratio is 60:25:15 gypsum/aluminum sulfate/aluminum oxide.By grinding
Raw meal powder afterwards is calcined at 1500 DEG C, and is incubated 30min at such a temperature, and insulation takes out firing sample in sky immediately after terminating
Quenching in gas, grinding to fineness is 360m2Calcium oxide expansive clinker is made in/kg.
Obtained calcium oxide expansive clinker is added into tetrahydrofuran of the number-average molecular weight for 10kg/mol polyacrylic acid
In solution, the mass ratio of calcium oxide and polyacrylic acid is 95:5, remove solvents tetrahydrofurane after mixing, gained solid through grinding extremely
Specific surface area is 250m2/ kg, packs and obtains modified oxidized calcium class cement concrete swelling agent 4 of the present invention.
As a comparison, the calcium oxide expansive clinker of above-mentioned long time without surface modification is labeled as 4 '.
Embodiment 5
It is 96 by mass ratio:It is through ball mill intergrinding to fineness after 4 lime stone and composite mineralizer mixing
260m2/ kg raw meal powder, wherein composite mineralizer are that mass ratio is 70:20:10 gypsum/aluminum oxide/aluminum sulfate.By grinding
Raw meal powder afterwards is calcined at 1200 DEG C, and is incubated 240min at such a temperature, and insulation is taken out firing sample after terminating and existed immediately
Quenching in air, grinding to fineness is 260m2Calcium oxide expansive clinker is made in/kg.
It is the four of 2kg/mol PVP that obtained calcium oxide expansive clinker is added into number-average molecular weight
In hydrogen tetrahydrofuran solution, the mass ratio of calcium oxide and PVP is 98:2, solvents tetrahydrofurane, institute are removed after mixing
It is 350m that solid, which is obtained, through grinding to specific surface area2/ kg, packs and obtains modified oxidized calcium class coagulating cement of the present invention
Soil expansion agent 5.
As a comparison, the calcium oxide expansive clinker of above-mentioned long time without surface modification is labeled as 5 '.
Embodiment 6
It is 95 by mass ratio:It is through ball mill intergrinding to fineness after 5 lime stone and composite mineralizer mixing
360m2/ kg raw meal powder, wherein composite mineralizer are that mass ratio is 40:32:25 gypsum/aluminum oxide/aluminum sulfate.By grinding
Raw meal powder afterwards is calcined at 1350 DEG C, and is incubated 80min at such a temperature, and insulation takes out firing sample in sky immediately after terminating
Quenching in gas, grinding to fineness is 360m2Calcium oxide expansive clinker is made in/kg.
Obtained calcium oxide expansive clinker is added into number-average molecular weight molten for the toluene of 100kg/mol PEO
In liquid, the mass ratio of calcium oxide and PEO is 99:1, solvent toluene is removed after mixing, gained solid is through grinding to than table
Area is 550m2/ kg, packs and obtains modified oxidized calcium class cement concrete swelling agent 6 of the present invention.
As a comparison, the calcium oxide expansive clinker of above-mentioned long time without surface modification is labeled as 6 '.
With reference to standard GB/T 23439-2009, by the modified oxidized calcium class cement concrete swelling agent obtained by the present invention
1-6, and the quality such as the mode mixed within the calcium oxide expansive clinker 1 ' -6 ' of surface modification substitution cement total amount is not carried out
8%, comparative study 1-6, and 1 ' -6 ' the foster expansion effect of water under restrictive condition to cement mortar of surface modification is not carried out
Inhibition is shunk with drying, result of the test is shown in Table 1.
Table 1
As can be seen from Table 1, the cement mortar specimen of modified oxidized calcium class cement concrete swelling agent of the present invention is mixed
Limited expansion rate when water supports 7d is much larger than unmodified conventional expanded agent-calcium oxide expansive clinker, and water is supported after 7d in sky
When maintenance 21d is dried in gas, 1-6 mortar specimen still shows larger dilatancy.Therefore, using produced by the present invention
Modified oxidized calcium class cement concrete swelling agent has larger limitation expansion performance in water supports environment, and in desiccation
Environment in still have larger effective expansion.
Modified oxidized calcium class coagulating cement earth concrete prepared by admixture embodiment 1 is monitored in real time using the micro- calorimeters of TAM
The hydration heat speed of swelling agent 1 and corresponding non-modified swelling agent-calcium oxide expansive clinker 1 '.As a result as shown in Fig. 2 passing
The unmodified calcium oxide expansive clinker of system rapid aquation after adding water, rate of heat release reaches maximum during 1h, and this has confirmed calcium oxide
Class expansive clinker consumes substantial amounts of invalid expansion energy in the hydrated cementitious plastic stage.Modified oxidized calcium class cement of the present invention
Cement expansive material early stage not aquation, aquation reaches most fast after 2 hours, significantly extends hydration time up to one times or so,
Mean that its invalid expansion in concrete plastic stage can be reduced.
The portland cements of PII 42.5 produced using the south of the River- little Ye fields Cement Co., Ltd, fixing water-cement ratio is
0.35, by the modified oxidized calcium class cement concrete swelling agent 1-6 produced by the present invention, and the swollen of surface modification is not carried out
The 8% of the mass substitution cement total amounts such as swollen dose-calcium oxide expansive clinker 1 ' -6 ', the cement paste benchmark sample of swelling agent is not mixed
Represented with blank.Directly maintenance is (20 ± 1) DEG C, relative humidity (60 ± 5) % drying contractile ring in temperature after specimen molding
In border, it is stripped after (24 ± 2) h and measures the piece lengths in just length, the certain curing age of one step surveying of going forward side by side.Dry to shrink and become
Form quotient is represented with linear deformation rate, wherein generating dilatancy, negative value on the occasion of concrete paste specimen under expression drying condition
Represent that concrete paste specimen generates contraction distortion under drying condition, result of the test is as shown in figures 3-8.
As a result show, mix the modified oxidized calcium class cement concrete swelling agent concrete paste specimen produced by the present invention
Obvious dilatancy can be produced early stage maintenance is dried, and there is significant compensating action to the contraction in later stage, compared to
Unmodified calcium oxide expansive clinker, dilatancy increased.
Claims (3)
1. a kind of modified oxidized calcium class cement concrete swelling agent, it is characterised in that the modified oxidized calcium class cement concrete
Swelling agent is made up of water soluble polymer organic polymer and calcium oxide expansive clinker, the water soluble polymer organic polymer
Thing is wrapped in the surface of calcium oxide expansive clinker；The specific surface area of the modified oxidized calcium class cement concrete swelling agent is
100-600m2/kg；
The water soluble polymer organic polymer accounts for the modified oxidized calcium class cement concrete swelling agent quality total amount
1%-20%；
The number-average molecular weight of the water soluble polymer organic polymer is 1-500kg/mol；Selected from polyacrylamide, poly- methyl
The mixture of one kind and any of the above ratio in acrylic acid, polyacrylic acid, PVP, PEO；
The preparation method of described modified oxidized calcium class cement concrete swelling agent, comprises the steps：
Macromolecule organic polymer anhydrous organic solvent is dissolved, the calcium oxide expansive clinker for adding metering is well mixed,
Residual organic solvents are removed, grinding to specific surface area is 100-600m2/kg；Produce the modified oxidized calcium class cement concrete
Swelling agent；
The anhydrous organic solvent is one in dry dichloromethane, chloroform, tetrahydrofuran, acetone, toluene, dimethylbenzene
Plant any of the above scalemic thereof.
2. modified oxidized calcium class cement concrete swelling agent according to claim 1, it is characterised in that the calcium oxide
The specific surface area of swelling agent clinker is 100-600m2/ kg, wherein free calcium oxide content (f-CaO) >=60%.
3. modified oxidized calcium class cement concrete swelling agent according to claim 1, it is characterised in that the calcium oxide
Expansive clinker is formed into calcining grinding at 1200-1500 DEG C after raw material by lime stone and composite mineralizer combined grinding, and it compares
Surface area is 100-600m2/kg；
Wherein the mass ratio of composite mineralizer and lime stone is 0:100~10:90；
Composite mineralizer by mass percentage content be 40%-100% gypsum, 0%-60% aluminum oxide and/or aluminum sulfate
Composition.
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| CN105198266A (en) * | 2015-11-01 | 2015-12-30 | 刘应才 | Anti-frost-crack concrete expansive agent and preparation method thereof |
| US10737981B2 (en) * | 2016-10-12 | 2020-08-11 | United States Gypsum Company | Method for making a lightweight gypsum composition with internally generated foam and products made from same |
| CN109574537B (en) * | 2017-09-28 | 2021-08-10 | 厦门凯景实业有限公司 | Self-waterproof concrete expanding agent and preparation method thereof |
| 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 |
| CN108483979A (en) * | 2018-04-04 | 2018-09-04 | 刘凡领 | A kind of cement waterproof agent |
| CN108328961B (en) * | 2018-04-18 | 2020-07-24 | 水利部交通运输部国家能源局南京水利科学研究院 | Modified calcium oxide expanding agent with controllable expansion process and preparation method thereof |
| CN109704623A (en) * | 2018-11-21 | 2019-05-03 | 南京工业大学 | A kind of MgO expansion agent and its preparation method and application that in-situ polymerization surface is modified |
| CN109851278B (en) * | 2019-03-27 | 2021-07-13 | 常熟京常智能科技有限公司 | Traffic detection equipment wall fixing expanding agent and preparation method thereof |
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| JPH10251043A (en) * | 1997-03-10 | 1998-09-22 | Ryoko Sekkai Kogyo Kk | Modified calcium oxide composition and its production |
| JP2003128449A (en) * | 2001-10-19 | 2003-05-08 | Denki Kagaku Kogyo Kk | Cement admixture, cement composition and concrete using the same |
| CN102674738A (en) * | 2012-05-09 | 2012-09-19 | 江苏博特新材料有限公司 | Multifunctional anti-crack additive |
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| CN101333083A (en) * | 2008-08-05 | 2008-12-31 | 中国建筑材料科学研究总院 | High performance expansible cement clinker expansion agent series prepared thereby |
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| JPH01208317A (en) * | 1987-10-20 | 1989-08-22 | Seii Kogyo Kk | Control of slaking reaction time of quick lime |
| JPH10251043A (en) * | 1997-03-10 | 1998-09-22 | Ryoko Sekkai Kogyo Kk | Modified calcium oxide composition and its production |
| JP2003128449A (en) * | 2001-10-19 | 2003-05-08 | Denki Kagaku Kogyo Kk | Cement admixture, cement composition and concrete using the same |
| CN102674738A (en) * | 2012-05-09 | 2012-09-19 | 江苏博特新材料有限公司 | Multifunctional anti-crack additive |
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