CN108424023B - Hydrophobic material and preparation method and application thereof - Google Patents
Hydrophobic material and preparation method and application thereof Download PDFInfo
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- CN108424023B CN108424023B CN201810353868.8A CN201810353868A CN108424023B CN 108424023 B CN108424023 B CN 108424023B CN 201810353868 A CN201810353868 A CN 201810353868A CN 108424023 B CN108424023 B CN 108424023B
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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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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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
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/04—Portland cements
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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
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/60—Agents for protection against chemical, physical or biological attack
- C04B2103/65—Water proofers or repellants
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/27—Water resistance, i.e. waterproof or water-repellent materials
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention provides a preparation method of a hydrophobic material, which comprises the following steps: calcining the Fenton paper-making sludge to obtain Fenton paper-making sludge ash; and ball-milling the Fenton paper-making sludge ash and stearic acid to obtain the hydrophobic material. When the doping amount of the hydrophobic material prepared by the invention reaches 4%, the compressive strength is 2.5MPa higher than that of a blank cement sample; when the doping amount of the hydrophobic material reaches 16%, the contact angle between a water drop and the set cement is 102 degrees. After the hydrophobic material is compounded with materials such as cement, the composite material is applied to waterproof projects such as a top plate, a floor slab, side slope sprayed concrete, a waterproof curtain and the like of an underground station, the erosion effect of water migration on the projects can be reduced, and a technical route for recycling Fenton paper-making sludge ash is provided.
Description
Technical Field
The invention relates to the technical field of sludge building materials, in particular to a hydrophobic material and a preparation method and application thereof.
Background
The discharge amount of the papermaking sludge in China is the first in the world, more than 2000 million tons of the papermaking sludge are discharged every year, and the papermaking sludge is mainly treated by landfill and fluidized bed high-temperature calcination. Land is occupied by landfill, so that land resource waste is caused; the calcined sludge has pozzolanic activity and can replace part of the cement clinker, and it has been confirmed by many studies that the us and uk research institutes have been studying it as an admixture to improve the properties of cement-based materials. Because of the increasing environmental requirements, large-scale paper mills generally require the use of fluidized bed processes, and the amount of calcined sludge produced thereby increases year by year. The reasonable recycling of the papermaking byproducts is an environmental protection problem which is urgently needed to be solved by the current society.
The transport of water in the pores of concrete is the main cause of deterioration of its properties. The treatment of the water leakage in civil engineering needs a large amount of capital and sometimes delays the construction period. Ordinary cement-based materials widely used in civil engineering have hydrophilic properties and are treated mainly by applying a waterproof coating or laying a waterproof film when used under water or in a wet environment. Under the action of power or alternating load, once the waterproof layer is damaged, the concrete structure loses the barrier and is easy to deteriorate. The development of compact cement-based materials with strong waterproof performance is an effective way to solve the problem, and the development of simple and rapid additives is particularly important.
Zhang Ru (Zhang Ru, Korea Cynanchum, Qianwei, Lisi, Tong Mei. preliminary study on surface modification and action mechanism of papermaking sludge [ J ] Chinese papermaking, 2014,33(01):15-19.) et al propose that the surface of papermaking wet sludge and diluent of various modifiers can generate hydrophobic groups after a hydrothermal method is carried out on the raw materials, wherein stearic acid has high modification activation index and can improve the compatibility with organic high polymers. Hong S.Wang (Hong S.Wong, Robert Baraka, Alhilai, et al.Hydrophobic sludge using water slurry [ J ]. Cement and Cement Research,2015, 70:9-20.) proposes that the paper making sludge ash of a newsprint factory is ball-milled and modified with stearic acid and added into Cement materials for use, thereby improving the mechanical properties of the materials and also improving the hydrophobicity. Disclosure of inventiontechnical problemmans 36191, et al (hole 36191, lisson, korean gold dragon. experimental study on the influence of surfactant modified metakaolin on cement performance [ J ]. novel building materials, 2015,42(12):60-62.) propose that a mixture obtained by ball-milling modification of metakaolin and stearic acid can be mixed into mortar to improve the fluidity thereof and remarkably improve the mortar strength.
Fenton paper sludge is H2O2And Fe2+The sludge treated by the strong oxidant contains higher iron content except the components of the conventional papermaking sludge. According to the literature, reasonable calcination is expected to improve the activity of Fenton paper-making sludge, and the feasibility of generating a hydrophobic material by ball milling modification with stearic acid is strong.
Disclosure of Invention
The invention aims to provide a preparation method of a hydrophobic material, so that the preparation process of the hydrophobic material is simplified, the mechanical property and the hydrophobic property of the hydrophobic material are improved, and a feasible technical route is provided for resource utilization of papermaking sludge.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a hydrophobic material, which comprises the following steps:
calcining the Fenton paper-making sludge to obtain Fenton paper-making sludge ash;
and ball-milling the Fenton paper-making sludge ash and stearic acid to obtain the hydrophobic material.
Preferably, the calcining temperature is 800-1000 ℃, and the calcining time is 1.5-2.5 h.
Preferably, the weight ratio of the stearic acid to the Fenton paper making sludge ash is 1: 24-25.
Preferably, the rotation speed of the ball milling is 350-.
The invention provides the hydrophobic material prepared by the preparation method in the technical scheme.
Preferably, the hydrophobic material comprises Al as a component2O3Calcium aluminoferrite, calcium silicate, wollastonite and gehlenite.
Preferably, the pH value of the water solution of the hydrophobic material is 11.0-12.0.
Preferably, the particle size of the hydrophobic material is 75 μm or less.
The invention provides the application of the hydrophobic material in the technical scheme in cement-based hydrophobic materials and concrete.
The invention provides a preparation method of a hydrophobic material, which comprises the following steps: calcining the Fenton paper-making sludge to obtain Fenton paper-making sludge ash; and ball-milling the Fenton paper-making sludge ash and stearic acid to obtain the hydrophobic material. According to the invention, stearic acid is doped to modify Fenton paper sludge through ball milling mechanical activation, on one hand, the paper sludge ash active components are metakaolin and Al2O3、CaCO3A large number of active hydroxyl groups on the surface and stearic acid are subjected to elimination reaction to generate C ≡ C, C-O-C or lipid hydrophobic groups, and simultaneously the surface energy is reduced, and the active hydroxyl groups can be uniformly distributed in an interface transition region of hardened cement stone and aggregate in hydration reaction; on the other hand, C formed by calcination2A large amount of inert particles such as F and the like can play a nucleation role in hydration, and the generated C-S-H gel can be clustered on the surfaces of the particles to compact the interface, so that the strength of the concrete is improved.
According to the invention, through heat treatment, Fenton paper-making sludge has certain volcanic ash activity and a micro-aggregate filling effect in cement application, hydrophobic groups are formed on the surface of the sludge ash after modification by stearic acid, and water drops are dropped into the hydrophobic materials to form a ball shape and are impermeable, so that the dispersibility is good, the agglomeration phenomenon is avoided in the stirring of ordinary portland cement, and the mechanical property and the hydrophobic property of the fenton paper-making sludge are improved. According to the data of the embodiment, when the cement replacement amount of the hydrophobic material prepared by the invention reaches 4%, the compressive strength reaches 73.08MPa, which is 2.5MPa higher than that of a blank cement sample 71.53MPa, and the contact angle and the water absorption rate are not obviously changed; when the doping amount of the hydrophobic material reaches 16%, the compressive strength of 61.43MPa is reduced by 10.1MPa compared with 71.53MPa of a blank cement sample, the contact angle between water drops and a cement stone is 102%, and the water absorption rate of 1.8% is reduced by 2% compared with 3.8% of the blank cement sample. After the hydrophobic material is compounded with materials such as cement, the composite material is applied to waterproof projects such as a top plate, a floor slab, side slope sprayed concrete, a waterproof curtain and the like of an underground station, the erosion effect of water migration on the projects can be reduced, and a technical route for recycling Fenton paper-making sludge ash is provided.
Detailed Description
The invention provides a preparation method of a hydrophobic material, which comprises the following steps:
calcining the Fenton paper-making sludge to obtain Fenton paper-making sludge ash;
and ball-milling the Fenton paper-making sludge ash and stearic acid to obtain the hydrophobic material.
The Fenton paper-making sludge is calcined to obtain the Fenton paper-making sludge ash. In the present invention, the temperature of the calcination is preferably 800-1000 ℃, more preferably 850 ℃ and 950 ℃, said calcination time preferably being between 1.5 and 2.5h, more preferably between 1.8 and 2.2 h. The invention leads the compound containing Fe, Al, Si and Ca in the sludge to generate melting composite reaction from the horn-shaped protruding block body by calcination to generate a calcium-iron-aluminum phase composite and amorphous SiO2、Al2O3The fine granular particles are obviously increased, the surface is smooth, and the fine granular particles can achieve a good modification effect with stearic acid under the condition of mechanical ball milling, so that the hydrophobicity is greatly improved.
After the Fenton paper making sludge ash is obtained, the Fenton paper making sludge ash and stearic acid are subjected to ball milling to obtain the hydrophobic material. In the present invention, the weight ratio of stearic acid to fenton paper sludge ash is preferably 1: 24-25. In the invention, the rotation speed of the ball milling is preferably 350-. The ball milling method is not particularly limited, and the ball milling method can be selected from the methods well known to those skilled in the art.
The invention provides the hydrophobic material prepared by the preparation method in the technical scheme. In the present invention, the composition of the hydrophobic material preferably includes Al2O3Calcium aluminoferrite, calcium silicate, wollastonite and gehlenite. Wherein wollastonite and Al2O3The surface of the modified aggregate has a large amount of active hydroxyl groups, and hydrophobic groups of lipids, such as-C ═ O and-CH, can be obtained on the surface after modification by stearic acid, can reduce the agglomeration phenomenon among mixtures, and are dispersed in an interface transition region of slurry and aggregate to block the migration and infiltration of water so as to achieve a hydrophobic effect; in the hydration with cement, the gehlenite and the calcium aluminoferrite are slowly hydrated, so that the hardened slurry structure becomes compact, a better gelling effect is generated, and the water absorption of the set cement is reduced. In the present invention, the pH of the hydrophobic material is preferably 11.0 to 12.0. In the present invention, the particle size of the hydrophobic material is 75 μm or less.
The invention provides the application of the hydrophobic material in the technical scheme in cement-based hydrophobic materials and concrete.
In the invention, the application method of the hydrophobic material in the cement-based hydrophobic material comprises the following steps:
mixing a hydrophobic material, ordinary portland cement and polypropylene fibers to obtain a mixed material;
and (3) adding water and stirring uniformly after the mixed materials are stirred until the polypropylene fibers are dispersed uniformly and do not agglomerate, thereby obtaining the cement-based hydrophobic material.
In the invention, the Portland cement is PO 42.5 Portland cement, and the mass ratio of the hydrophobic material, the water and the Portland cement is preferably 5-19: 7-35: 20-100 parts of; the polypropylene fiber is preferably 19mm long, the slenderness ratio is 380, and the tensile strength is 358 MPa; the mass ratio of the polypropylene fibers to the hydrophobic material is preferably 2-3: 1000.
in the invention, the application method of the hydrophobic material in concrete comprises the following steps:
mixing hydrophobic materials, ordinary portland cement, stones and sand to obtain dry-mixed materials;
and mixing the mixed solution of the polycarboxylic acid water reducing agent and water with the dry-mixed material to obtain the concrete.
In the present invention, the ordinary portland cement is preferably PO 42.5 portland cement; the pebbles are preferably pebbles with the particle size of 10-16mm and 16-20mm, and the mass ratio of the pebbles with the particle size of 10-16mm and the particle size of 16-20mm is preferably 7: 3. In the invention, the sand is preferably river sand, and the configuration fineness modulus is 2.8. In the present invention, the water reducing rate of the polycarboxylic acid water reducing agent is preferably 20%. In the present invention, the mass ratio of the water, the ordinary portland cement, the sand, and the stones is preferably 14: 27-29: 47: 100. in the invention, the mass ratio of the hydrophobic material to the ordinary portland cement is preferably 1-9: 24-100, the mass ratio of the polycarboxylic acid water reducing agent to the hydrophobic material is preferably 7: 50-100.
The following examples are provided to illustrate the preparation of a hydrophobic material of the present invention in detail, but they should not be construed as limiting the scope of the present invention.
Example 1
Calcining the Fenton paper-making sludge at 1000 ℃ for 2.5h to obtain Fenton paper-making sludge ash; after cooling, the Fenton papermaking sludge ash and stearic acid are uniformly mixed according to the weight ratio of 24:1, and then ball milling is carried out for 6 hours under the condition that the rotating speed is 350r/min, so as to obtain the hydrophobic material. The particle size of the obtained hydrophobic material is 45-75 μm and accounts for 99.87%, and the particle size below 45 μm and accounts for 0.13%.
Example 2
Calcining the Fenton paper-making sludge at 800 ℃ for 2.5h to obtain Fenton paper-making sludge ash; after cooling, the Fenton paper making sludge ash and stearic acid are uniformly mixed according to the weight ratio of 25:1, and then ball milling is carried out for 6 hours under the condition that the rotating speed is 380r/min, so as to obtain the hydrophobic material. The detection shows that the particle size of the obtained hydrophobic material is 45-75 μm accounting for 89.36%, and the particle size below 45 μm accounting for 10.64%.
Example 3
Uniformly mixing the hydrophobic material prepared in the example 1, ordinary portland cement and polypropylene fibers according to a mass ratio to obtain a mixed material; stirring the mixed materials until the polypropylene fibers are uniformly dispersed and not agglomerated, adding water and stirring uniformly to obtain the cement-based hydrophobic material; wherein, the mass ratio of the hydrophobic material to the water to the ordinary portland cement is 19: 35: 100, respectively; the mass ratio of the polypropylene fiber to the hydrophobic material is 3: 1000.
the cement-based hydrophobic material is blended and molded into a prism test block with the thickness of 40mm multiplied by 160mm, the actual measurement compressive strength after demoulding standard curing for 28d is 59.02MPa, the breaking strength is 7.59MPa, the water absorption is 1.81 percent, and the contact angle between water drops at the middle fracture surface and the set cement is 102 degrees.
Example 4
Uniformly mixing the hydrophobic material prepared in the example 1, ordinary portland cement and polypropylene fibers according to a mass ratio to obtain a mixed material; stirring the mixed materials until the polypropylene fibers are uniformly dispersed and not agglomerated, adding water and stirring uniformly to obtain the cement-based hydrophobic material; wherein, the mass ratio of the hydrophobic material to the water to the ordinary portland cement is 5: 7: 20; the mass ratio of the polypropylene fiber to the hydrophobic material is 2: 1000.
the cement-based hydrophobic material is blended and molded into a prism test block with the thickness of 40mm multiplied by 160mm, the actual measurement compressive strength after demoulding standard curing for 28d is 53.75MPa, the breaking strength is 6.56MPa, the water absorption is 2.74 percent, and the contact angle between water drops at the middle fracture surface and the set cement is 116 degrees.
Example 5
Mixing the hydrophobic material prepared in the embodiment 2, ordinary portland cement, stones and sand to obtain a dry mixture; mixing the mixed solution of the polycarboxylic acid water reducing agent and water with the dry-mixed material to obtain concrete; wherein the mass ratio of the water to the ordinary portland cement to the sand to the stones is 14: 27: 47: 100, respectively; the mass ratio of the hydrophobic material to the ordinary portland cement is 9: 100, the mass ratio of the polycarboxylic acid water reducing agent to the hydrophobic material is 7: 100.
the concrete is blended and molded into a cube test block with the thickness of 100mm multiplied by 100mm, the actual measurement compressive strength after demolding and standard curing for 28d is 43.68MPa, the splitting tensile strength is 1.97MPa, and the average growth rate of the capillary water absorption height in unit area in 1d is 0.352 mm/h.
Example 6
Mixing the hydrophobic material prepared in the embodiment 2, ordinary portland cement, stones and sand to obtain a dry mixture; mixing the mixed solution of the polycarboxylic acid water reducing agent and water with the dry-mixed material to obtain concrete; wherein the mass ratio of the water to the ordinary portland cement to the sand to the stones is 14: 29: 47: 100, respectively; the mass ratio of the hydrophobic material to the ordinary portland cement is 1:24, the mass ratio of the polycarboxylic acid water reducing agent to the hydrophobic material is 7: 50.
the concrete is blended and molded into a cube test block with the size of 100mm multiplied by 100mm, the actual measurement compressive strength after demolding and standard curing for 28d is 39.73MPa, the splitting tensile strength is 1.87MPa, and the average growth rate of the capillary water absorption height in unit area in 1d is 0.416 mm/h.
From the above examples, the present invention provides a method for preparing a hydrophobic material, comprising the following steps: calcining the Fenton paper-making sludge to obtain Fenton paper-making sludge ash; and ball-milling the Fenton paper-making sludge ash and stearic acid to obtain the hydrophobic material. According to the invention, through heat treatment, Fenton paper-making sludge has certain volcanic ash activity and a micro-aggregate filling effect in cement application, hydrophobic groups are formed on the surface of the sludge ash after modification by stearic acid, and water drops are dropped into the hydrophobic materials to form a ball shape and are impermeable, so that the dispersibility is good, the agglomeration phenomenon is avoided in the stirring of ordinary portland cement, and the mechanical property and the hydrophobic property of the fenton paper-making sludge are improved. According to the data of the embodiment, when the doping amount of the hydrophobic material prepared by the invention reaches 4%, the compressive strength is 2.5MPa higher than that of a blank cement sample; when the doping amount of the hydrophobic material reaches 16%, the contact angle between a water drop and the set cement is 102 degrees. After the hydrophobic material is compounded with materials such as cement, the composite material is applied to waterproof projects such as a top plate, a floor slab, side slope sprayed concrete, a waterproof curtain and the like of an underground station, the erosion effect of water migration on the projects can be reduced, and a technical route for recycling Fenton paper-making sludge ash is provided.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A method of preparing a hydrophobic material, comprising the steps of:
calcining the Fenton paper-making sludge to obtain Fenton paper-making sludge ash;
and ball-milling the Fenton paper-making sludge ash and stearic acid to obtain the hydrophobic material.
2. The preparation method as claimed in claim 1, wherein the calcination temperature is 800-1000 ℃ and the calcination time is 1.5-2.5 h.
3. The method according to claim 1, wherein the weight ratio of stearic acid to fenton's paper sludge ash is 1: 24-25.
4. The preparation method as claimed in claim 1, wherein the rotation speed of the ball mill is 350-400r/min, and the ball milling time is 4-6 h.
5. A hydrophobic material prepared by the preparation method of any one of claims 1 to 4.
6. The hydrophobic material of claim 5, wherein the composition of the hydrophobic material comprises Al2O3Calcium aluminoferrite, calcium silicate, wollastonite and gehlenite.
7. The hydrophobic material according to claim 6, wherein the hydrophobic material and the water are mixed in a mass ratio of 1: 10, and the pH value of the water solution after centrifugation is 11.0-12.0.
8. The hydrophobic material according to claim 7, wherein the particle size of the hydrophobic material is 75 μm or less.
9. Use of the hydrophobic material of any one of claims 5 to 8 in a cement-based hydrophobic material or concrete;
the application method of the hydrophobic material in the cement-based hydrophobic material comprises the following steps:
mixing a hydrophobic material, ordinary portland cement and polypropylene fibers to obtain a mixed material;
and (3) adding water and stirring uniformly after the mixed materials are stirred until the polypropylene fibers are dispersed uniformly and do not agglomerate, thereby obtaining the cement-based hydrophobic material.
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| CN101386690B (en) * | 2008-10-22 | 2011-01-19 | 中山大学 | Waste paper sludge composite filler and preparation method and application thereof |
| CN101941815B (en) * | 2010-08-19 | 2012-08-15 | 俞锡贤 | Activated modified water repellent agent and preparation method thereof |
| GB201410030D0 (en) * | 2014-06-05 | 2014-07-16 | Imp Innovations Ltd | Hydrophobic powder |
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| CHARACTERIZATION AND DEWATERING OF ACTIVATED SLUDGE DEWATERING OF ACTIVATED SLUDGE FROM THE PULP AND PAPER INDUSTRY;J Pere 等;《Water Science & Technology》;19931212;第193-201页 * |
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