CN108218274A - Improve inorganic dispersant of geo-polymer slurry rheology energy and its preparation method and application - Google Patents
Improve inorganic dispersant of geo-polymer slurry rheology energy and its preparation method and application Download PDFInfo
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- CN108218274A CN108218274A CN201810095913.4A CN201810095913A CN108218274A CN 108218274 A CN108218274 A CN 108218274A CN 201810095913 A CN201810095913 A CN 201810095913A CN 108218274 A CN108218274 A CN 108218274A
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- geo
- polymer slurry
- inorganic dispersant
- preparation
- fly ash
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
- C04B22/0006—Waste inorganic materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/40—Surface-active agents, dispersants
- C04B2103/408—Dispersants
Abstract
The present invention provides a kind of inorganic dispersants for improving geo-polymer slurry rheology energy and its preparation method and application, are related to the production preparation field of construction material.The preparation method of the inorganic dispersant includes：Fly ash grain and lye are mixed and are incorporated at 50~80 DEG C after 1~6h of stirring, then fly ash grain with the solution containing low-surface energy substance is mixed and 0.5~1.5h is impregnated at 55~65 DEG C.The inorganic dispersant prepared by this method has hydrophobic surface, and ' ball ' effect can be played in high alkalinity and highly viscous geo-polymer slurry, reduces plastic viscosity, improves the rheological property of geo-polymer slurry.
Description
Technical field
The present invention relates to the production preparation field of construction material, in particular to a kind of improvement geo-polymer slurry
Inorganic dispersant of rheological property and its preparation method and application.
Background technology
Geo-polymer is one kind by activated aluminum siliceous raw material (metakaolin, flyash and slag etc.) and alkali-activator
React the green phosphor cementitious material prepared.Geo-polymer has the excellent specific properties such as early strong, fine and close and corrosion-resistant, and can high level
Change using trade waste, therefore have broad application prospects in the special engineerings such as Rapid-Repair and fixed-end forces field.
However, the preparation process due to geo-polymer need to have highly basic using what sodium hydroxide and waterglass configuration formed
Property and highly viscous solution be exciting agent, this causes the rheological characteristic of geo-polymer slurry poor, and workability is difficult to control.It is conventional
The macromolecule dispersing agents such as naphthalene system, lignosulfonates and polycarboxylic acids for portland cement sill are in geo-polymer slurry
In produce little effect, and both at home and abroad not yet prepare can be effectively improved geo-polymer slurry rheology can mating additive.This
Great difficulty is brought to the molding and pumping operation of slurry, seriously affects the application popularization of geology polymer material.
Invention content
The purpose of the present invention is to provide a kind of inorganic dispersants and its system for improving geo-polymer slurry rheology energy
Preparation Method and application, this inorganic dispersant have hydrophobic surface, can be starched in high alkalinity and highly viscous geo-polymer
' ball ' effect is played in body, reduces plastic viscosity, improves the rheological property of geo-polymer slurry.
In order to realize the above-mentioned purpose of the present invention, spy uses following technical scheme：
A kind of preparation method for the inorganic dispersant for improving geo-polymer slurry rheology energy, including：
Fly ash grain and lye are mixed and are incorporated at 50~80 DEG C after 1~6h of stirring, then by fly ash grain with containing
The solution mixing of low-surface energy substance simultaneously impregnates 0.5~1.5h at 55~65 DEG C.
One kind inorganic dispersant as made from above-mentioned preparation method.
A kind of application of above-mentioned inorganic dispersant in geo-polymer slurry rheology energy is improved.
Compared with prior art, beneficial effects of the present invention for example including：
1. existing macromolecule dispersing agent produces little effect in high alkalinity and highly viscous geo-polymer slurry, and this hair
It is bright to make public for the first time a kind of inorganic dispersant for improving geo-polymer slurry rheology energy, the nothing handled through super hydrophobic surface
Machine dispersant can significantly improve the rheological property of geo-polymer slurry, contribute to the popularization and application of geology polymer material.
2. this inorganic dispersant using the not wettability of fly ash grain super hydrophobic surface, gives full play to flyash
" ball " effect and space steric effect of particle reduce the particle in high alkalinity and highly viscous geo-polymer slurry environment
Between Surface adhesion force, avoid particle agglomeration, reduce the plastic viscosity of slurry, and then play diminishing and peptizaiton, improve ground
The rheological property of matter polymer slurry.
3. the flyash that the present invention selects is common building material, cheap, the chemical etching of inorganic dispersant is prepared
And the serial of methods such as surface low energyization modification are easy to operate, preparation process is easy to spread.
Description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described.
Fig. 1 is the fly ash grain after surface roughening treatment；
Fig. 2 is the fly ash grain after sieving and ultrasonic cleaning.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific
Condition person, the condition suggested according to normal condition or manufacturer carry out.Reagents or instruments used without specified manufacturer is
The conventional products that can be obtained by commercially available purchase.
Applicants have found that by being mixed in cement-based material with the fly ash grain of ball-type pattern, can play " ball "
Effect reduces the frictional dissipation between cement granules, improves slurry rheology energy.However, by fly ash grain incorporation geology polymerization
But without apparent peptizaiton in object slurry.Applicant's process carefully analyzes and persistent exploration, finds this is because fly ash grain
After being contacted with highly viscous alkali-activator, the frictional resistance mutually moved between particle is excessively high, leads to not play " ball " effect.
Therefore, in order to play " ball " effect of fly ash grain in geo-polymer slurry, present embodiment provides
A kind of inorganic dispersant, this inorganic dispersant are handled by chemical etching and surface hydrophobicity, made using fly ash grain as raw material
Fly ash grain has hydrophobic surface, and then reduces the plastic viscosity of geo-polymer slurry, improves geo-polymer slurry
Rheological property.
Present embodiment also provides the preparation method of the inorganic dispersant of this improvement geo-polymer slurry rheology energy,
It includes：
Step S1. chemical etchings：Fly ash grain and lye are mixed and are incorporated in 1~6h of stirring at 50~80 DEG C.
Fly ash grain is mixed with lye, and at 50~80 DEG C (or at 60~70 DEG C；Or at 63~68 DEG C)
It is stirred continuously carry out chemical etching, construction coarse particles surface.Fly ash microsphere after etching as shown in Figure 1, microsphere surface
Nano level particle and bowl configurations are formd, the wettability of fly ash microsphere in the liquid phase can be reduced.
Further, lye is that a concentration of 5-10mol/L is either 6~9mol/L or is 7~8mol/L.The powder
The solid-to-liquid ratio of coal ash particle and the lye is 1：25~35 or for 1：26~34；Or it is 1：28~32；Or it is 1：29
~31.Preferably, lye is NaOH solution or KOH solution.
Further, the grain size of fly ash grain is less than 80 μm, and more preferably, grain size is 60~80 μm or is 65
~75 μm.The fly ash grain of this grain size is obtained by the way that level-one flyash to be crossed to the square hole screen of 180 mesh or so.First level flour
Coal ash is common building material, cheap.Fly ash grain in 70~90 μm of particle size ranges can preferably play " rolling
Pearl " effect and space steric effect help further to improve the rheological characteristic of geo-polymer slurry.
Further, fly ash grain further includes the step of being cleaned with alcoholic solution before being mixed with the lye.Compared with
It to be preferred, is mixed using by fly ash grain with ethanol solution, the method being cleaned by ultrasonic.Cleaning and dried fine coal
As shown in Fig. 2, being ultrasonically treated the attachment of microsphere surface capable of washing, raising surface flatness is conducive in flyash grey microballoon
Particle surface does hydrophobically modified.
The processing of step S2. surface hydrophobicities：Fly ash grain is mixed with the solution containing low-surface energy substance and in 55~
0.5~1.5h is impregnated at 65 DEG C.
The fly ash microsphere of roughening treatment is mixed with the prepared solution containing low-surface energy substance, in 55~65
Dipping 0.5~1.5 (or 0.8~1.2h is impregnated at 57~63 DEG C), carries out low energy surface modification, makes rough surface at DEG C
Fly ash microsphere have hydrophobic surface, so as to have superhydrophobic characteristic.
Further, low-surface energy substance includes 17 fluorine decyl trimethoxy silanes, 17 fluorine decyl triethoxysilicanes
Alkane, tridecafluoro-n-octyltriethoxysilane and 1H, 1H, 2H are one or more in 2H-perfluoro capryl trichlorosilane.
Further, a concentration of 0.7 of low-surface energy substance described in the solution containing the low-surface energy substance
~1.3wt% is either 0.8~1.2wt% or is 0.9~1.1wt%.
Further, the solvent in the solution containing the low-surface energy substance is in ethyl alcohol, methanol and propyl alcohol
At least one more preferably, uses ethyl alcohol as solvent.
Further, further including will be dry under oxygen-free environment of the fly ash grain at 100~110 DEG C after dipping
1.5~2.5h.Wherein, oxygen-free environment is the environment under nitrogen or inert gas shielding.More preferred, drying steps are：
By 1.8~2.2h dry under nitrogen environment of the fly ash grain at 103~107 DEG C after dipping.
Present embodiment also provides a kind of application of inorganic dispersant in geo-polymer slurry rheology energy is improved,
Including：Above-mentioned inorganic dispersant is mixed by the amount of mixing of 2~8wt% with the geo-polymer slurry.
Further, geo-polymer slurry is by that will have the powder material of pozzolanic activity and liquid exciting agent
(mixture of NaOH and waterglass, modulus are 1.5~1.7) is according to mass ratio 1:0.8~1.2 is mixed 80~120s systems
.Wherein, the powder material with pozzolanic activity is the one or more of flyash, granulated blast-furnace slag and metakaolin.
Such inorganic dispersant is mixed, using the not wettability of the super hydrophobic surface of fly ash grain, gives full play to powder
" ball " effect and space steric effect of coal ash particle reduce the intergranular table in high viscosity geo-polymer slurry environment
Face viscous force avoids particle agglomeration, reduces the plastic viscosity of geo-polymer slurry, and then plays diminishing and peptizaiton, changes
The rheological property of kind slurry.
The feature and performance of the present invention are described in further detail with reference to embodiments：
Embodiment 1
The present embodiment provides a kind of inorganic dispersant for improving geo-polymer slurry rheology energy, preparation method packets
It includes：
Level-one flyash is crossed into 180 mesh square hole screens, takes and tails over to obtain the ball-type fly ash grain that grain size is less than 80 μm.By powder
Coal ash particle is mixed with ethanol solution to be cleaned by ultrasonic, with NaOH solution (8mol/L) by 1 after cleaning:30 solid-to-liquid ratio is mixed
It closes, 3h is stirred under 50 DEG C of hydrothermal conditions and carries out chemical etching, construction coarse particles surface.
Using ethyl alcohol as solvent, the 17 fluorine decyl trimethoxies that 17 fluorine decyl trimethoxy silanes are configured to 1wt% are added in
Base silane/ethanol solution.The fly ash grain of roughening treatment with prepared solution is mixed, impregnates 1h at 60 DEG C, into
Row low energy surface modification.N of the microballoon at 105 DEG C after dipping22h is dried under environment, obtains inorganic dispersant.
By flyash and liquid exciting agent (mixture of NaOH and waterglass, modulus 1.6) in mass ratio 1:1 mixing,
Fly ash base geo-polymer slurry is made in stirring 100s.Obtained inorganic dispersant is polymerize by 2% volume with geology
Object slurry mixes, and stirs 60s mixings.Using slurry plastic viscosity before and after the such dispersant of rotational viscometer comparison measuring and calculating incorporation
Variation.Geo-polymer slurry is shaped to test specimen, standard curing 28d after form removal, analysis dispersant is to hardenite mechanical property
Influence.
Embodiment 2
The present embodiment provides a kind of inorganic dispersant for improving geo-polymer slurry rheology energy, preparation method packets
It includes：
Level-one flyash is crossed into 180 mesh square hole screens, takes and tails over to obtain the spherical particles that grain size is less than 80 μm.By flyash
Grain is mixed with ethanol solution and is cleaned by ultrasonic, with the NaOH solution of 10mol/L that has been configured by 1 after cleaning:30 solid-to-liquid ratio
Mixing stirs 2h under 70 DEG C of hydrothermal conditions and carries out chemical etching, construction coarse particles surface.
Using ethyl alcohol as solvent, 17 fluorine decyl, three ethoxy that 17 fluorine decyl triethoxysilanes are configured to 1wt% is added in
The fly ash grain of roughening treatment with prepared solution is mixed, impregnates 1h at 60 DEG C by base silane/ethanol solution, into
Row low energy surface modification.N of the fly ash grain at 105 DEG C after dipping22h is dried under environment, inorganic dispersant is made.
By metakaolin and liquid exciting agent (mixture of NaOH and waterglass, modulus 1.6) in mass ratio 1:1 is mixed
It closes, metakaolin base geological polymer slurry is made in stirring 100s.Inorganic dispersant is starched by 8% volume with geo-polymer
Body mixes, and stirs 60s mixings.The change of slurry plastic viscosity before and after the such dispersant of measuring and calculating incorporation is compared using rotational viscometer
Change.Geo-polymer slurry is shaped to test specimen, standard curing 28d after form removal, analysis dispersant is to hardenite mechanical property
It influences.
Embodiment 3
The present embodiment provides a kind of inorganic dispersant for improving geo-polymer slurry rheology energy, preparation method packets
It includes：
Level-one flyash is crossed into 180 mesh square hole screens, takes and tails over to obtain the spherical particles that grain size is less than 80 μm.By flyash
Grain is mixed with ethanol solution and is cleaned by ultrasonic, with the NaOH solution of 5mol/L that has been configured by 1 after cleaning:30 solid-to-liquid ratio is mixed
It closes, 6h is stirred under 60 DEG C of hydrothermal conditions and carries out chemical etching, construction coarse particles surface.
Using ethyl alcohol as solvent, ten trifluoro octyl groups, three ethoxy that tridecafluoro-n-octyltriethoxysilane is configured to 1wt% is added in
The fly ash grain of roughening treatment with prepared solution is mixed, impregnates 1h at 60 DEG C by base silane/ethanol solution, into
Row low energy surface modification.N of the microballoon at 105 DEG C after dipping22h is dried under environment, inorganic dispersant is made.
By granulated blast-furnace slag and liquid exciting agent (mixture of NaOH and waterglass, modulus 1.6) in mass ratio 1:1
Slag base geological polymer slurry is made in mixing, stirring 100s.By volume and geo-polymer slurry of the inorganic dispersant by 8%
60s mixings are stirred in mixing.The variation of slurry plastic viscosity before and after the such dispersant of measuring and calculating incorporation is compared using rotational viscometer.
Geo-polymer slurry is shaped to test specimen, standard curing 28d after form removal, analysis dispersant is to the shadow of hardenite mechanical property
It rings.
The rheological property analysis of 1 geo-polymer of experimental example
At 20 DEG C, before and after rotational viscometer (Chandler-Model 3530) comparison measuring and calculating incorporation inorganic dispersant
The variation of geo-polymer slurry plastic viscosity.
The shear stress of rotor slurry under 3/6/10/20/30/60/100/200/300/600rpm rotating speeds is read, is used
Bingham model (formula 1) is fitted data, and the plastic viscosity of slurry is calculated.
τ=τ0+ηγ (1)
Wherein τ is shear stress, and γ is shear rate, τ0For yield strength, η is plastic viscosity.
Table 1 illustrate the geo-polymer slurry of embodiment 1-3 offers plastic viscosity and it is corresponding do not mix it is inorganic
The plastic viscosity of the control sample of dispersant.
The comparative analysis of 1 geo-polymer slurry plastic viscosity of table
The experimental results showed that for the geo-polymer of three kinds of matrixes such as flyash, metakaolin and slag, powder is mixed
The plastic viscosity of slurry reduces 73.5%, 70.7% and 73.3% respectively after inorganic dispersant.Thus illustrate, such dispersant
Good diminishing peptizaiton has been played in high alkalinity and highly viscous geo-polymer slurry, has effectively improved the stream of slurry
Become performance.
The intensity test of 2 geo-polymer hardenite of experimental example
Using geo-polymer hardenite resistance to compression before and after WHY-200 type universal testing machines measurement of comparison incorporation inorganic dispersant
The variation of intensity.
Pressure resistance is carried out after the square geo-polymer test specimen mark that size is 30mm × 30mm × 30mm is supported 28d ages
Degree test, loading speed 0.5mm/min.It is averaged after 6 test blocks of every group of sample testing.
Table 2 illustrates the compression strength of the geo-polymer hardenite of embodiment 1-3 offers and corresponding does not mix nothing
The compression strength of the control sample of machine dispersant.
The comparative analysis of 2 geo-polymer hardenite compression strength of table
The experimental results showed that for the geo-polymer of three kinds of matrixes such as flyash, metakaolin and slag, incorporation is inorganic
The compression strength of dispersant after-hardening body is without being substantially reduced, therefore strength development of this inorganic dispersant to geology polymer material
It has no adverse effect.
Although illustrate and describing the present invention with specific embodiment, it will be appreciated that without departing substantially from the present invention's
Many other change and modification can be made in the case of spirit and scope.It is, therefore, intended that in the following claims
Including belonging to all such changes and modifications in the scope of the invention.
Claims (10)
1. a kind of preparation method for the inorganic dispersant for improving geo-polymer slurry rheology energy, which is characterized in that it includes：
Fly ash grain and lye are mixed and are incorporated at 50~80 DEG C after 1~6h of stirring, then by the fly ash grain with containing
The solution mixing of low-surface energy substance simultaneously impregnates 0.5~1.5h at 55~65 DEG C.
2. the preparation method of the inorganic dispersant according to claim 1 for improving geo-polymer slurry rheology energy,
It is characterized in that, the low-surface energy substance includes 17 fluorine decyl trimethoxy silanes, 17 fluorine decyl triethoxysilanes, ten
Trifluoro octyltri-ethoxysilane and 1H, 1H, 2H are one or more in 2H-perfluoro capryl trichlorosilane.
3. the preparation method of the inorganic dispersant according to claim 1 for improving geo-polymer slurry rheology energy,
Be characterized in that, low-surface energy substance described in the solution containing the low-surface energy substance a concentration of 0.7~
1.3wt%.
4. the preparation method of the inorganic dispersant according to claim 1 for improving geo-polymer slurry rheology energy,
It is characterized in that, the solvent in the solution containing the low-surface energy substance is at least one of ethyl alcohol, methanol and propyl alcohol.
5. the preparation method of the inorganic dispersant according to claim 1 for improving geo-polymer slurry rheology energy,
It is characterized in that, the lye is a concentration of 5-10mol/L, and the solid-to-liquid ratio of the fly ash grain and the lye is 1：25~
35。
6. the preparation method of the inorganic dispersant according to claim 1 for improving geo-polymer slurry rheology energy,
It is characterized in that, the fly ash grain further includes the step of being cleaned with alcoholic solution before being mixed with the lye.
7. the preparation method of the inorganic dispersant according to claim 1 for improving geo-polymer slurry rheology energy,
Be characterized in that, further include will dry 1.5 under oxygen-free environment of the fly ash grain at 100~110 DEG C after dipping~
2.5h。
8. a kind of inorganic dispersant as made from claim 1~7 any one of them preparation method.
9. a kind of application of inorganic dispersant according to claim 8 in geo-polymer slurry rheology energy is improved.
10. application according to claim 9, which is characterized in that the inorganic dispersant by 2~8wt% the amount of mixing with
The geo-polymer slurry mixing.
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Cited By (1)
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| CN113999553A (en) * | 2021-11-11 | 2022-02-01 | 中国矿业大学 | Fly ash-based super-hydrophobic coating and preparation method thereof |
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