CN114772967B - Artificial granite waste residue reinforced aggregate, pervious concrete and preparation method and application thereof - Google Patents
Artificial granite waste residue reinforced aggregate, pervious concrete and preparation method and application thereof Download PDFInfo
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- CN114772967B CN114772967B CN202210323765.3A CN202210323765A CN114772967B CN 114772967 B CN114772967 B CN 114772967B CN 202210323765 A CN202210323765 A CN 202210323765A CN 114772967 B CN114772967 B CN 114772967B
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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
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/10—Coating or impregnating
- C04B20/1018—Coating or impregnating with organic materials
- C04B20/1029—Macromolecular compounds
- C04B20/1033—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00241—Physical properties of the materials not provided for elsewhere in C04B2111/00
- C04B2111/00284—Materials permeable to liquids
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
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- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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Abstract
The invention discloses an artificial granite waste residue reinforced aggregate, a pervious concrete and a preparation method and application thereof, and the preparation method comprises the following steps: drying and grinding the artificial granite waste residue into coarse grinding materials, then mixing the coarse grinding materials with a grinding aid, a dispersing agent and water for ball milling, and drying the ball milling materials to obtain a powdery finished product; mixing the powdery finished product and an acrylic acid solution for reaction for a set time, and drying to obtain powder; adding water into the powder for dispersion, and adding an initiator, an accelerator and a cross-linking agent into the powder to prepare a calcium acrylate polymer solution; soaking diabase aggregate in calcium acrylate polymer solution for a set time, taking out, wrapping cement, and drying to obtain the aggregate.
Description
Technical Field
The invention belongs to the technical field of solid waste utilization, and particularly relates to an artificial granite waste residue reinforced aggregate, a permeable concrete and a preparation method and application thereof.
Background
The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art.
Artificial granite is also called synthetic stone, reconstructed stone and engineering stone. The building stone slab is a synthetic stone which is made by using natural marble crushed aggregates and granite white mud as main raw materials and adding organic resin as a cementing agent through the processes of vacuum stirring, high-pressure vibration forming, room-temperature curing and the like, and is cut into a building material stone slab, and is widely applied to the building decoration industry. The artificial granite slab has various and rich colors, the generated waste residues have different colors, and the white mud of solid wastes contains more unsaturated polyester resin, residual alkali, soluble salts such as iron, potassium, magnesium and the like and impurities, is difficult to be used as a filler of products such as paint, coating and the like, cannot be treated and can only be stacked. The stone waste residue has great harm to the environment and is difficult to degrade in a short time. After the rock waste residue stacking body is infiltrated into rainwater for multiple times, the clay in the rock-soil mixture can be softened after absorbing water and expanding, the consolidation capability between the clay and the rock is lost due to water absorption, and the stability is gradually reduced. So that a slope debris flow can be formed to cause disastrous results. The stone waste residue can cause groundwater pollution after being soaked by rainwater, and raise dust can be formed in good weather, so that air pollution is caused.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide an artificial granite waste residue reinforced aggregate, a pervious concrete, and a preparation method and application thereof.
In order to realize the purpose, the invention is realized by the following technical scheme:
in a first aspect, the invention provides a preparation method of an artificial granite waste residue reinforced aggregate, which comprises the following steps:
drying and grinding the artificial granite waste residue into coarse grinding materials, then mixing the coarse grinding materials with a grinding aid, a dispersing agent and water for ball milling, and drying the ball milling materials to obtain a powdery finished product;
mixing the powdery finished product and an acrylic acid solution for reaction for a set time, and drying to obtain powder;
adding water into the powder for dispersion, and adding an initiator, an accelerator and a cross-linking agent into the powder to prepare a calcium acrylate polymer solution;
soaking diabase aggregate in calcium acrylate polymer solution for a set time, taking out, wrapping cement, and drying to obtain the aggregate.
In a second aspect, the invention provides an artificial granite waste residue reinforced aggregate prepared by the preparation method.
In a third aspect, the invention provides pervious concrete, which comprises aggregate, cement, a water reducing agent and water, wherein the aggregate is the artificial granite waste residue reinforced aggregate.
The beneficial effects achieved by one or more of the embodiments of the invention described above are as follows:
the strength of the pervious concrete after setting and hardening mainly comes from mutual embedding and mechanical meshing among aggregate particles on one hand, and from the interface bonding strength between the aggregate surface and a cementing material on the other hand. In addition to the strength and firmness of the coarse aggregate, the particle size and shape, the surface characteristics and impurities, the strength of the weaker interfacial transition zone between the coarse aggregate and the cementitious material is a key factor in the influence of the mechanical and water permeability properties of pervious concrete. The transition area of the aggregate particle-cement interface determines the mechanical property, corrosion resistance, water permeability resistance and the overall characteristics of the pervious concrete to a greater extent, and is one of the most important factors influencing the service life of the pervious concrete.
The permeable concrete aggregate pretreatment solution formed by grinding the artificial granite waste residue and chemically treating the artificial granite waste residue by adopting the acrylic acid solution can improve the bonding strength of a permeable concrete diabase-cement interface transition region, and further improve the strength and durability of permeable concrete.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a diagram of an apparatus for preparing an artificial granite waste residue calcium polyacrylate solution, b is a photograph of an artificial granite waste residue calcium polyacrylate solution soaked in diabase aggregate, c is a photograph of diabase aggregate soaked and strengthened by the artificial granite waste residue calcium polyacrylate solution, d is a photograph of diabase aggregate soaked and strengthened by wrapping a certain amount of cement and air-drying, e is a photograph of formed permeable concrete after soaking and strengthening of diabase aggregate, f is a test diagram of permeability of the formed permeable concrete, and g is a test diagram of mechanical properties of the formed permeable concrete; h is a state diagram after the forming of the pervious concrete is broken;
FIG. 2 is an FTIR spectrum of glauconite aggregates of different treatments, wherein A0 is unmodified glauconite aggregate, A1 is modified glauconite aggregate, and A1c is glauconite aggregate coated with a cement layer;
FIG. 3 is an XRD pattern of cement hydrates at different ages of modified and unmodified diabase aggregates;
fig. 4 is XRD patterns of cement hydrates at different ages of unmodified and modified diabase aggregates, wherein (a) is SEM micrograph (10000 times) of unmodified diabase aggregates at 3d age; (b) Is an SEM micro-morphology picture (10000 times) of the 3d age of the modified diabase aggregate; (c) Is an SEM micro-morphology picture (5000 times) of an unmodified diabase aggregate at the 3d age; (d) Is an SEM micro-morphology picture (5000 times) of the 3d age of the modified diabase aggregate; (e) SEM micrograph of unmodified diabase aggregate at 28d age (5000 x); (f) An SEM microtopography (5000 times) of 28 d-age modified diabase aggregate;
FIG. 5 is a graph comparing the effect of sodium Polyacrylate (PAAS) loading and calcium acrylate concentration at 3d age on pH;
FIG. 6 is a graph comparing the effect of sodium Polyacrylate (PAAS) loading at 7d age and calcium acrylate concentration on pH;
FIG. 7 shows the shape of the pervious concrete before and after aggregate pretreatment, (a) pretreated diabase pervious concrete (sample # 4); and (b) is blank diabase pervious concrete (sample # 0).
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
In a first aspect, the invention provides a preparation method of an artificial granite waste residue reinforced aggregate, which comprises the following steps:
drying and grinding the artificial granite waste residue into coarse grinding materials, then mixing the coarse grinding materials with a grinding aid, a dispersing agent and water for ball milling, and drying the ball milling materials to obtain a powdery finished product; mixing the powdery finished product and an acrylic acid solution for reaction for a set time, and drying to obtain powder;
adding water into the powder for dispersion, and adding an initiator, an accelerator and a cross-linking agent into the powder to prepare a calcium acrylate polymer solution;
soaking diabase aggregate in calcium acrylate polymer solution for a set time, taking out, wrapping cement, and drying to obtain the aggregate.
Because the artificial granite takes the crushed natural marble as the main raw material and contains the organic resin cementing agent, the powder is milled into powder and dried, which is beneficial to the dispersion of calcium carbonate and organic resin, and is further beneficial to the mixing and dissolving in the solution and the subsequent reaction with acrylic acid.
In some embodiments, the grinding aid is prepared by a method comprising the following steps: reacting maleic anhydride and triethanolamine under the catalytic action of p-toluenesulfonic acid to obtain an intermediate monomer RM;
carrying out dropwise free radical copolymerization on the intermediate monomer RM, maleic anhydride, methyl allyl polyoxyethylene ether, a main monomer, an initiator and a chain transfer agent, and adjusting a reaction system to be neutral after reacting for a set time to obtain the intermediate monomer RM; the main monomer is Acrylic Acid (AA) or itaconic acid.
Preferably, the initiator is ammonium persulfate.
Preferably, the chain transfer agent is sodium methallyl sulfonate.
The mixing amount of the synthetic grinding aid is 0.02-0.03 percent.
In some embodiments, the dispersant is a mixture of sodium lignosulfonate and a polycarboxylic acid high-efficiency water reducing agent, and the mass ratio of the sodium lignosulfonate to the polycarboxylic acid high-efficiency water reducing agent is 3:5-9, preferably 3:7. The mixing amount of the dispersant is 0.08-0.10%.
In some embodiments, the mass ratio of coarse abrasive to grinding aid to dispersant to water is 60 to 70:2 to 3: 8-10: 25 to 35.
In some embodiments, the final powder obtained after ball milling has a particle size of 45 μm to 75 μm.
Preferably, the time for mixing and reacting the powdery finished product and the acrylic acid solution is 30-40min. The artificial granite contains organic resin cementing agent such as unsaturated polyester resin, cyclohexanone peroxide and the like, and the substances can be subjected to graft copolymerization or coating in a calcium polyacrylate solution in the processes of calcium polyacrylate polymerization generation and branched chain enlargement after grinding.
In some embodiments, the acrylic acid concentration is 99.5% to 100%.
Preferably, the initiator is a protic initiator such as sulfuric acid or a free radical initiator such as ammonium persulfate or potassium persulfate.
Preferably, the accelerator is one or a mixture of several of reducing agent, alcohol, ketone, ester, ether, phenol, inorganic phosphide, organic phosphine, organic amine and organic acid. Such as triisopropanolamine, triethanolamine.
Preferably, the crosslinking agent is butyl acrylate, hydroxyethyl acrylate, hydroxypropyl acrylate, hydroxyethyl methacrylate or hydroxypropyl methacrylate.
In some embodiments, the diabase aggregate is soaked in the calcium acrylate polymer solution for a period of 10 to 30min, preferably 15 to 25min.
Preferably, after the diabase aggregate is soaked, a layer of cement paste is wrapped.
Further preferably, the thickness of the diabase-coated cement paste after air-drying is 0.05-0.15 mm.
In a second aspect, the invention provides an artificial granite waste residue reinforced aggregate prepared by the preparation method.
In some embodiments, the particle size of the artificial granite waste slag-reinforced aggregate is 4 to 10mm.
In a third aspect, the invention provides pervious concrete, which comprises aggregate, cement, a water reducing agent and water, wherein the aggregate is the artificial granite waste residue reinforced aggregate.
In some embodiments, the mass ratio of aggregate, cement, water reducer and water is 1000-2000:500-600:1-2:100-200.
According to the method, the aggregate particles are soaked in the calcium polyacrylate solution with different concentrations through chemical pretreatment, the bonding strength of a permeable concrete diabase-cement interface transition region is improved, and the influence of diabase aggregate pretreatment on the mechanical strength and the water permeability of the permeable concrete is researched. The present invention will be further described with reference to the following specific examples.
Raw material
Cement: P.O 42.5.5 grade ordinary portland cement, produced by Guangxi Huarun cement, inc., the main chemical components are shown in Table 1, and the physical and mechanical performance indexes are shown in Table 2;
aggregate: diabase macadam, produced by diabase mining ltd, east county, guangxi, the chemical element analysis results of the aggregate are shown in Table 3, and the physical performance indexes are shown in Table 4;
the waste residue of artificial granite is taken from a production line of a large artificial granite in Hehe of Guangxi, and the analysis results of XRD and XRF chemical components are respectively shown in table 1 and figure 2.
Acrylic acid: analytical purity of Shanghai Mielin Biochemical technology Co., ltd;
triethanolamine: the Shanghai national drug group chemical reagent company Limited produces, and the analysis is pure;
butyl acrylate: analytical purity of Shanghai Mielin Biochemical technology Co., ltd;
water reducing agent: the self-made polycarboxylic acid high-performance water reducing agent has the water reducing rate of 30 percent and the solid content of 39.6 percent.
TABLE 1 chemical element analysis results of artificial granite waste (unit:%)
TABLE 2 index of physical and mechanical properties of cement
TABLE 3 index of physical Properties of aggregate
TABLE 4 aggregate chemical element analysis results TABLE (unit:%)
Test method
Drying and grinding white mud of an artificial granite solid waste, which is taken back by enterprises in the gigayuan industry demonstration base of calcium carbonate in Kyoho Guangxi, into coarse grinding materials, 2000g of the coarse grinding materials, 60g of grinding aids and 180g of a polycarboxylic acid high-efficiency water reducing agent (PCE) serving as a dispersing agent, adding 820g of water, putting the mixture into a ball mill for ball milling for 120min, filtering to obtain a liquid finished product, and drying to obtain a powdery finished product.
The preparation method of the grinding aid comprises the following steps: maleic Anhydride (MAH), triethanolamine (the molar ratio of 2:1) and p-toluenesulfonic acid (catalyst) are used as raw materials, and the reaction is carried out for 2.5 hours at 105 ℃, so as to obtain an intermediate monomer RM. Then, the intermediate monomer RM, maleic Anhydride (MAH), methallyl polyoxyethylene ether (TPEG), acrylic Acid (AA) (main monomer), ammonium persulfate (initiator) and sodium methallyl sulfonate (SMAS) (chain transfer agent) are subjected to dropwise free radical copolymerization synthesis under an initiation system of 60-70 ℃, wherein RM: AA: TPEG molar ratio 1.5: 1.2: 1, the amount of chain transfer agent (SMAS) and initiator (ammonium persulfate) used was 2.5% and 1.0% by mass of TPEG, respectively. After reacting for 3.5 hours, adjusting the pH value of NaOH solution to about 7 to obtain the artificial granite waste residue grinding aid RMJ. The Acrylic Acid (AA) may be replaced by itaconic acid.
Placing 1000g of the dried and ground powdery finished product and 1500g of acrylic acid in a beaker with a continuous stirrer in a fume hood, reacting for 40min, filtering the solution, and drying in vacuum to obtain solid powder.
Dissolving a certain amount of the solid powder in water, preparing a certain volume of solution with different concentrations by adopting an orthogonal test method under the condition of different mixing amounts of an initiator, an accelerator and a cross-linking agent, soaking diabase aggregate particles in a container for 20min, taking out the diabase aggregate particles, sieving, wrapping a certain amount of cement, and performing air drying for 24h for later use, wherein the table 5 shows the results. The blank control was soaked in water, coated with the same cement and air dried.
The thickness of the coating of the slurry. Selecting aggregate particles with approximate spherical shape, and the dried aggregate particles have mass m 1 The polymer slurry is uniformly coated on the surface of the aggregate, and the mass of the aggregate is m when the aggregate is maintained by covering a film at normal temperature 2 Then, the thickness of the wrapping layer is calculated according to the following formula:
in the formula: h-thickness/mm of the wrapping layer of the slurry; rho-density of the slurry, g/cm 3 ；
s-surface area of coarse aggregate, mm 2 。
Setting the solution configuration concentration and the doping amount (based on the mass of potassium persulfate, triethanolamine and butyl acrylate) of potassium persulfate, triethanolamine and butyl acrylate as investigation factors, taking the compressive strength and the water permeability coefficient of the aggregate-formed water-permeable concrete 7d and 28d after the polymer solution is soaked as investigation indexes, selecting three levels on each factor, and performing four-factor three-level orthogonal experiments, wherein the L9 (34) factor level is shown in Table 5.
TABLE 5 levels of orthogonal test factors
TABLE 6 test mix proportions of pervious concrete
The test mix proportion of the pervious concrete is shown in table 6, after the pervious concrete is formed by vibration of a 30L single-horizontal-shaft forced mixer and is subjected to standard curing for a certain age, the 3d, 7d and 28d compressive strength and the water permeability coefficient of each group of samples are tested, and the influence of the calcium acrylate pretreated aggregate on the mechanical property and the water permeability of the pervious concrete is researched.
During the water permeability test, firstly, the four side surfaces of the test piece are coated with solid butter, then, the test piece is sealed by using a waterproof adhesive tape, and then, the test piece is placed into a water permeability coefficient tester to ensure that no gap exists between the test piece and the inner wall of the water outlet, as shown in figure 1.
On the basis of the optimal factor combination, the changes of hydration reaction of the cement in the transition region of the aggregate interface and the appearance of the product are researched by respectively adopting analytical means such as FTIR, SEM, XRD and the like for the unmodified aggregate and the modified aggregate.
Results and analysis
Influence of artificial granite waste residue modified aggregate on permeable concrete performance
The influence of the calcium acrylate modified diabase aggregate on the performance of the pervious concrete is researched through an orthogonal test, and the orthogonal test design, the performance test result and the range analysis are shown in table 7.
TABLE 7L 16 (3 4 ) Orthogonal test design and performance test result and range analysis
Compared with an untreated sample, the early strength of the formed permeable concrete after the diabase aggregate is pretreated is reduced to different degrees, but the later strength is obviously improved, and the change of the water permeability is not obvious. The reason is probably that the calcium polyacrylate product formed on the surface of the aggregate has an internal network structure, absorbs a part of free water in the early stage of cement hydration, is fixed on a macromolecular chain in a manner of forming a hydrogen bond, reduces the evaporation of mixing water and has better water retention performance. However, the pervious concrete mainly utilizes the cement slurry to coat the aggregate to form a cementing layer, and the early hydration of the cement is influenced to a certain extent by reducing the water amount participating in the early hydration, so that the early mechanical property of the modified aggregate pervious concrete is influenced.
The data comparison shows that the 28d compressive strength of the 5# sample is the highest and is 34.8Mpa, which is improved by 21.2 percent compared with the blank group, the 7d compressive strength is reduced by 1.8 percent, and the water permeability coefficient is reduced by 4.1 percent compared with the blank group. The water permeability coefficient of the No. 6 sample is the highest and is 2.37mm/s, which is improved by 7.2 percent compared with that of a blank group. The extreme differences of all factors are analyzed, so that the influence of the concentration of the polymerized monomer calcium acrylate in the pretreatment solution on the mechanical property and the water permeability coefficient is the largest, the extreme differences of the polymerized monomer calcium acrylate in the pretreatment solution on the compressive strength of the 7d and 28d ages are the largest, and the concentration of the calcium acrylate in the pretreatment solution is the best 10% according to the change condition of the strength along with the factor level.
The butyl acrylate is used as a polymerization cross-linking agent, the mixing amount of the butyl acrylate also influences the mechanical property and the water permeability of the pervious concrete, wherein compared with the 7d compressive strength, the 28d compressive strength and the water permeability coefficient of the formed concrete are influenced more obviously, and the mixing amount of the cross-linking agent with the age of 28d is 15% from the use angle of the pervious concrete. The potassium persulfate is used as an initiator for the polymerization of calcium acrylate, and the influence of the addition amount on the compressive strength and the water permeability is smaller than that of other three factors. Meanwhile, the influence of the mixing amount of the polymerization reaction accelerant triethanolamine on the 28d compressive strength of the pervious concrete is larger than that of the pervious concrete with the 7d compressive strength, but the influence on the permeability coefficient is not obvious, so that the optimal mixing amount of the accelerant is 2.5 percent.
In summary, the optimal scheme is A2B3C3D2, namely the concentration of the calcium acrylate in the pretreatment solution is 10%, and the mixing amounts of the butyl acrylate, the potassium persulfate and the triethanolamine are respectively 15%, 2.5% and 2.5% based on the mass of the calcium acrylate. In conclusion, the concentration of calcium acrylate in the aggregate pretreatment solution is the main factor influencing the mechanical property of the formed pervious concrete, and the influence of the concentration of calcium acrylate and the doping amount of butyl acrylate on the compressive strength and the water permeability of the pervious concrete is more obvious along with the extension of the age.
FTIR test analysis of artificial granite waste residue modified aggregate
Infrared spectroscopy tests are respectively carried out on unmodified diabase aggregate A0, modified diabase aggregate A1 and modified diabase aggregate A1c coated with a certain amount of cement, morphological changes of calcium acrylate monomers and polymers formed on the surface of the modified diabase aggregate are researched, morphological changes of the polymers of the calcium acrylate monomers and the polymers on the surface of the modified diabase aggregate are compared, and FTIR test analysis results are shown in figure 2.
In an infrared spectrogram of the modified aggregate A1, 3700cm is obtained -1 ～3200cm -1 In the interval, a stretching vibration of a plurality of hydroxyl groups was observedKinetic absorption band, which indicates the simultaneous presence of-OH due to free and different associated forms. 1413cm -1 Is a COO-symmetric stretching vibration band, which proves the existence of carboxylate, 1639cm -1 And 852cm -1 Vibration absorption bands of upsilon C = C and delta C-H of vinyl respectively, 711cm -1 The absorption spectrum of (A) is the- (CH) n-vibration absorption band, 972cm -1 is-CH = CH 2 Indicating that the pretreated diabase aggregate surface contains unsaturated C = C double bonds of acrylic polymer. Meanwhile, it is also possible that the ground artificial granite waste residue can be subjected to graft copolymerization or coating of organic substances such as organic resin adhesives such as partially unsaturated polyester resin, cyclohexanone peroxide and the like in a calcium polyacrylate solution in the processes of calcium polyacrylate polymerization generation and branch chain enlargement, and the organic substances are subjected to soaking pretreatment and then exist on the surface of diabase aggregate.
The above infrared spectrum can also find 852cm -1 ，972cm -1 ，1782cm -1 The absorption band of the polymer disappears or weakens, which indicates that the calcium acrylate in the aggregate pretreatment solution is polymerized under the action of the auxiliary agent, and forms addition polymerization or coupling among chemical bonds to generate linear calcium acrylate polymer under the action of free radicals released by an initiator potassium persulfate. Under the action of a cross-linked bridge frame of butyl acrylate, a plurality of linear polymers are bonded and interwoven to form a multi-dimensional parallel net structure. The infrared spectrogram of the surface of diabase aggregate A1c coated with the cement is similar to the spectrogram of a sample A1 of the pretreated aggregate not coated with the cement, and as can be seen in the chart, the characteristic peak of the polymer on the surface of the aggregate coated with the cement is 2036cm -1 The absorption strength of the formed coupling double bond is less obvious and is 1413cm -1 Is a carboxylic acid salt COO-symmetrical telescopic vibration band, the absorption intensity of the COO-band after polymerization is weakened, 852cm -1 The absorption intensity of vinyl band is weakened because partial groups are covered after cement reacts with calcium polyacrylate and substances or after the reaction, so that the absorption peak of the groups is reduced, the polymerization speed of residual monomers can be accelerated by alkaline conditions, and Ca (OH) is generated after the cement is coated 2 The olefinic carboxylate is easy to react with free Ca under the action of alkali 2+ The absorption peak is lowered due to the formation of an unstable complex.
The coating of the silicate cement is proved to have no influence on the polymer form formed on the surface of the diabase aggregate by pretreatment, and the cement pores on the surface of the aggregate are filled by the coating of the calcium acrylate polymer on the surface of the aggregate and the modification polymerization of the silicate cement, so that the structure of the cement stone of the later cementing layer is compact, and weak factors for the damage of the pervious concrete are reduced.
XRD (X-ray diffraction) phase analysis of artificial granite waste residue modified aggregate
And analyzing crystalline substances in the surface hardening cement slurry of the molded unmodified diabase aggregate A0 and the modified diabase aggregate A1 by adopting an X-ray diffractometer. After standard curing to a certain age, removing the surface layer, crushing, taking the inner core of the cement slurry on the surface of the aggregate, stopping hydration, drying, grinding, sieving and testing, wherein the XRD diffraction spectrum result is shown in figure 3.
The main components of the ordinary portland cement clinker include tricalcium silicate, dicalcium silicate, tricalcium aluminate, tetracalcium aluminoferrite, calcium sulfate and the like. In the initial stage of hydration reaction, once the surface of cement particles is contacted with water, complex hydration reaction can be started, different cement hydration products are continuously generated, and the cement hydration products and cement clinker are gradually coexisted.
As shown in FIG. 3, ca (OH) is visible in the XRD pattern of 3d and 7d age cement hydrate 2 Diffraction peaks of phases such as ettringite (AFt) and C-S-H gel. 2 theta 18.0 DEG and 47.0 DEG is Ca (OH) 2 The XRD diffraction peak of the modified diabase aggregate A1, ca (OH) generated by cement hydration on the surface can be found by the XRD diffraction spectrogram of the cured 3d and 7d ages 2 The diffraction peak intensity is lower than that of the untreated aggregate A0, and the degree of reduction of the diffraction peak intensity of the modified sample surface cement in the 3d stage is more obvious.
Untreated sample 3d age C 3 S and C 2 The diffraction peak intensity of S is significantly higher than that of the modified sample, C 3 S and C 2 The diffraction peak intensity of S also shows that the early hydration reaction process of the ordinary portland cement clinker on the surface of the diabase aggregate sample after pretreatment is slowed down.
The difference of the diffraction peak intensities before and after the aggregate pretreatment proves that the calcium acrylate polymer in the pretreatment solution has certain influence on the cement hydration of the transition zone of the aggregate-cement interface, and combines the mechanical property and the infrared analysis result, which is considered to be due to the free Ca in the alkaline medium of the calcium acrylate polymer and the cement hydration product 2+ Formation of unstable complex, acceleration of C 3 S and C 2 Hydrolysis of S to precipitate Ca (OH) formed by nucleation 2 Produces certain side effects, the calcium acrylate polymerization product promotes the generation of early AFt, so that hydrated early Ca (OH) appears 2 The diffraction peak intensity is lower.
Meanwhile, the calcium acrylate polymer is polymerized into a film-forming adsorption layer in an aggregate-cement interface area to adsorb Ca in the early stage of hydration 2+ And water molecules diffuse to the surface of cement particles to generate adverse effects, and the steric hindrance effect is generated on the gel structure of a hydration product, so that the early mechanical property of the modified aggregate permeable concrete is lower than that of a blank sample. As can be seen from the XRD spectrogram of the cured 7d age, ca (OH) on the surface of the modified aggregate 2 The diffraction peak intensity was still lower than that of the blank but the decrease was not significant compared to 3d, indicating that the calcium acrylate polymer and Ca were present 2+ The formed complex is unstable and can be automatically decomposed along with the continuous progress of hydration reaction, the inhibition effect of the calcium acrylate polymer on the cement hydration reaction is continuously reduced, and the inhibition effect is probably only on the early hydration stage of the cement.
The diffraction peak intensity of the modified sample AFt is slightly higher than that of the blank cement, and the diffraction peak intensity of the AFm is slightly lower, so that the stability of the AFt is improved to a certain extent by calcium acrylate, the AFt is gradually controlled to be converted into the AFm, and the calcium acrylate polymer is presumed to play a certain promoting role in fully reacting silicate in the later stage of cement slurry in an interface transition zone on the surface of the aggregate, and the improvement of the strength of the pervious concrete is facilitated.
SEM analysis of hydrated cement compound in transition region on surface of artificial granite waste residue modified aggregate
After the surface hardening cement slurry of the non-modified diabase aggregate A0 and the modified diabase aggregate A1 in the age of 3d and 7d is hydrated, the diabase aggregate A0 and the modified diabase aggregate A1 are knocked into small sheet samples, the small sheet samples are sprayed with gold, the cross section morphology of the small sheet samples is subjected to SEM observation, and the micro morphology characteristics of cement hydration products at the aggregate-cement stone interface in different ages are analyzed, wherein FIG. 4 is an SEM micro morphology picture.
As shown in fig. 4, SEM photographs of the 3d hydration microstructures of the blank and the modified aggregate-cement interface cement hydrate show that a large amount of silicate hydrates begin to form at the initial stage of cement hydration, and the structures overlap and coexist, and that the pores in the hydrates partially form needle-shaped AFt crystals of axially-grown elongated rod-shaped crystals. When the scanning electron microscope is magnified by 10000 times and 5000 times, the sizes of the AFt crystals growing in the cement paste on the surface of the pretreated modified aggregate A1 are observed to be smaller than the size of the A0 sample, and the AFt crystals are mostly gathered in clusters in the development state.
Meanwhile, more C-S-H hydration product gel is generated in the pores of the A1 sample and is overlapped into a fine fiber shape, which shows that the appearance of the silicate hydration product in the interface transition region is influenced by the calcium acrylate polymer generated on the surface of the aggregate. As can be seen from the SEM photograph of the scanning electron microscope at the age of 28d under the condition of 5000 times magnification, the number of fibrous calcium monosulfo-sulphoaluminate clusters is reduced after the surface of the aggregate is modified by the calcium acrylate polymer. The cementing layer of the surface interface transition region of the pretreated aggregate A1 is improved, the structural gap formed by the surface and cement is less, and the compactness is higher. The modified sample C-S-H crystals are mutually overlapped and filled in cement pores, so that the compactness of cement is improved to a certain extent, the later strength of an aggregate-cement-stone interface transition region and the aggregate cementing capacity of pervious concrete are favorably influenced, the structure of the cement stone is more compact, and the defects of the pores, cracks and the like are fewer.
A cement glue junction area of the calcium acrylate polymer modified aggregate A1 is visible, a compact and smooth polymerization layer is formed between diabase aggregate and part of cement, and the calcium acrylate polymer formed on the surface of the aggregate A1 is possibly participated in a secondary hydration process of a silicate hydration product by combining the results of an FTIR (infrared spectroscopy) and an XRD (X-ray diffraction) diffraction spectrum before the polymerization, so that a gelled structure with irregular shape is formed, the improvement of the later strength of the transition area of the aggregate and the cement interface is accelerated, and therefore, a strength modified aggregate sample tested by a mechanical property test method 28d is higher than a blank aggregate sample. Meanwhile, the reduction of the early strength further shows that the calcium acrylate polymer has partial inhibition effect on the primary hydration of the portland cement clinker, but the later hydration of the cement is more sufficient, which is beneficial to the development of the later strength.
Results and discussion
The influence of the calcium acrylate pretreatment aggregate on the performance of the pervious concrete by adopting an orthogonal test method, the early strength of the pervious concrete with the pretreated aggregate is slightly reduced, the later strength is greatly improved, and the change of the water permeability is not obvious. Through orthogonal test data and range analysis, the concentration of calcium acrylate in the pretreatment solution is 10%, the doping amount of butyl acrylate is 15%, the doping amount of potassium persulfate is 2.5%, and the doping amount of triethanolamine is 2.0%. The 7d compressive strength of the optimal sample pervious concrete is reduced by 1.8 percent, the 28d compressive strength is 34.8MPa, the compressive strength is improved by 21.2 percent compared with a blank group, and the permeability coefficient is reduced by 4.1 percent compared with the blank group.
Infrared spectroscopic analysis proves that the pretreated aggregate surface has a characteristic peak of a functional group of a calcium acrylate polymer, which indicates that the calcium acrylate in the aggregate pretreatment solution generates a linear polymer through addition polymerization under the action of free radicals released by an initiator, and the linear polymer is bonded and crosslinked into a network structure under the bridging action of a crosslinking agent. After cement coating is added, ca (OH) is generated due to the cement coating 2 The olefinic carboxylate is easy to react with free Ca under the action of alkali 2+ An unstable complex is formed, and a partial absorption peak is lowered. The coating of the silicate cement is proved to have no influence on the form of the polymer formed on the surface of the diabase aggregate by pretreatment, and the cement pores on the surface of the aggregate are filled by the polymerization of the coating of the calcium acrylate polymer and the cement on the surface of the aggregate, so that the structure of the cement stone of the later cementing layer is compact, and weak damage factors of the pervious concrete are reduced.
XRD diffraction pattern shows that the pre-treated sample hydration early Ca (OH) 2 Lower diffraction peak intensity, free Ca in alkaline medium of calcium acrylate polymer and cement hydration product 2+ Formation of unstable complex, acceleration of C 3 S and C 2 Hydrolysis of S to precipitate Ca (OH) formed by nucleation 2 Certain side effects are generated, and the formation of early AFt is promoted by the calcium acrylate polymerization product. Third to fourthPolymerization of calcium enoate polymers at the aggregate-cement interface region for Ca at the early stage of hydration 2+ And water molecules are diffused to the surface of cement particles to generate adverse effects, and a steric hindrance is formed on the gel structure of a hydration product, so that the early strength of the modified aggregate permeable concrete is low.
SEM electron microscope observation shows that the AFt crystals growing in the cement slurry on the surface of the early-stage modified aggregate are small in size and mostly gather in a cluster shape in the development state, and meanwhile, more fine fibrous C-S-H hydration product gels exist in sample pores, which shows that the appearance of the silicate hydration product in the interface transition region is influenced by the calcium acrylate polymer generated on the surface of the aggregate. The calcium acrylate polymer formed on the surface of the modified aggregate participates in the secondary hydration process of silicate hydration products, a gelled structure with irregular shape is formed, the improvement of the later strength of the transition area of the aggregate and the cement interface is accelerated, and the later strength of the modified aggregate pervious concrete is improved.
The damage morphology of the pervious concrete after the 28d compressive strength test is shown in fig. 7, after the test piece is pressed and broken in the pressure test, more large-particle-size diabase aggregate fracture phenomena appear in a 4# modified solution pretreated diabase aggregate test piece in the graph (a) and compared with 0# blank diabase pervious concrete in the graph (b), the fracture surfaces of the 0# blank diabase pervious concrete during compression are all generated in the interface transition region of large-particle-size diabase aggregate-cement paste, and the fact that the fracture surfaces have acted in the 28d age period is also explained from the other aspect, so that the mechanical property of the pretreated aggregate pervious concrete is continuously improved along with the increase of the age period.
Furthermore, the pretreated aggregate is doped with sodium Polyacrylate (PAAS) solid white powder to prepare a plant-growing concrete matrix, the pH value of the environment in the foam concrete is adjusted within a certain age period, and the feasibility of the aggregate concrete as the plant-growing matrix after the acrylic acid modified artificial granite waste residue polymer is pretreated is explored.
The pretreated aggregate is mixed with sodium Polyacrylate (PAAS) solid white powder to prepare the plant-growing concrete matrix. Can reduce early alkalinity of pervious concrete, and sodium Polyacrylate (PAAS) is a super absorbent resin with ultrahigh relative molecular mass, is mainly used as a water absorbent and has high water retention. The plant growth substrate has the advantages of repeatability of releasing and absorbing, strong water storage capacity and contribution to meeting the plant growth requirement. The strength of the plant-growing concrete matrix prepared from the pretreated aggregate is improved, the pH value is reduced, and the plant growth is facilitated. The pH value test method adopts a solid-liquid extraction method. Crushing the sample prepared in the test, fully grinding and sieving, weighing 10g, adding 10 times of distilled water by mass, plugging by a rubber plug, uniformly vibrating, filtering by filter paper after 2h, and testing the pH value of the filtrate by an acidimeter.
As can be seen from FIGS. 5 and 6, the pH values of the blank groups 3d and 7d of the green concrete samples prepared by using the pretreated aggregate are higher than that of the permeable concrete sample prepared by using the calcium polyacrylate solution to pretreat the aggregate and mix with the sodium polyacrylate. In the blank, the pH of the modified sample filtrate decreased with increasing calcium acrylate concentration in the pretreatment solution. Meanwhile, after the sodium polyacrylate is further doped, the pH value of the permeable concrete sample filtrate is reduced more obviously. The concentration of the pretreated calcium acrylate is 15%, and the pH value of the filtrate of the 3d pervious concrete sample prepared by blending the pervious concrete with 0.1% of sodium polyacrylate (by weight of cement) is 10.3, so that the optimal condition is achieved. The modified aggregate is doped with the sodium polyacrylate, so that the pH value in the pervious concrete can be reduced to a certain extent, and the mechanical property is improved compared with that of a blank sample. Feasibility of using aggregate concrete as a plant growth matrix after acrylic acid modified artificial granite waste residue polymer pretreatment.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of artificial granite waste residue reinforced aggregate is characterized by comprising the following steps: the method comprises the following steps:
drying and grinding the artificial granite waste residue into coarse grinding materials, then mixing the coarse grinding materials with a grinding aid, a dispersing agent and water for ball milling, and drying the ball milling materials to obtain a powdery finished product;
mixing the powdery finished product and an acrylic acid solution for reaction for a set time, and drying to obtain powder;
adding water into the powder for dispersion, and adding an initiator, an accelerator and a cross-linking agent into the powder to prepare a calcium acrylate polymer solution;
soaking diabase aggregate in the calcium acrylate polymer solution for a set time, taking out, wrapping cement, and drying to obtain the aggregate;
the preparation method of the grinding aid comprises the following steps: reacting maleic anhydride and triethanolamine under the catalytic action of p-toluenesulfonic acid to obtain an intermediate monomer RM;
carrying out dropwise free radical copolymerization on the intermediate monomer RM, maleic anhydride, methyl allyl polyoxyethylene ether, a main monomer, an initiator and a chain transfer agent, and adjusting a reaction system to be neutral after reacting for a set time to obtain the intermediate monomer RM;
the dispersing agent is a mixture of sodium lignosulfonate and a polycarboxylic acid high-efficiency water reducing agent, and the mass ratio of the sodium lignosulfonate to the polycarboxylic acid high-efficiency water reducing agent is 3:5-9;
the mass ratio of the coarse grinding material to the grinding aid to the polycarboxylic acid water reducing agent to water is 60 to 70:2~3:8 to 10:25 to 35.
2. The method for preparing the artificial granite waste residue reinforced aggregate as claimed in claim 1, which is characterized in that: the main monomer is acrylic acid or itaconic acid;
the initiator is ammonium persulfate;
the chain transfer agent is sodium methyl propylene sulfonate.
3. The method for preparing the artificial granite waste residue reinforced aggregate as claimed in claim 1, characterized in that: the dispersing agent is a mixture of sodium lignosulfonate and a polycarboxylic acid high-efficiency water reducing agent, and the mass ratio of the sodium lignosulfonate to the polycarboxylic acid high-efficiency water reducing agent is 3:7; the mixing amount of the dispersant is 0.08 to 0.10 percent.
4. The method for preparing the artificial granite waste residue reinforced aggregate as claimed in claim 1, which is characterized in that: the particle size of a powdery finished product obtained after ball milling is 45-75 mu m;
the time for mixing and reacting the powdery finished product and the acrylic acid solution is 30-40min.
5. The method for preparing the artificial granite waste residue reinforced aggregate as claimed in claim 1, characterized in that: the concentration of the acrylic acid solution is 99.5% -100%;
the initiator is a proton type initiator or a free radical initiator;
the accelerant is one or a mixture of a plurality of reducing agents, alcohol, ketone, ester, ether, phenol, inorganic phosphide, organic phosphine, organic amine and organic acid;
the cross-linking agent is butyl acrylate, hydroxyethyl acrylate, hydroxypropyl acrylate, hydroxyethyl methacrylate or hydroxypropyl methacrylate.
6. The method for preparing the artificial granite waste residue reinforced aggregate as claimed in claim 1, which is characterized in that: the diabase aggregate is soaked in the calcium acrylate polymer solution for 10-30min, and a layer of cement paste is wrapped after the diabase aggregate is soaked.
7. The method for preparing the artificial granite waste residue reinforced aggregate as claimed in claim 1, characterized in that: soaking diabase aggregate in the calcium acrylate polymer solution for 15-25min;
the thickness of the diabase-wrapped cement paste after air drying is 0.05 to 0.15mm.
8. An artificial granite waste residue reinforced aggregate is characterized in that: prepared by the preparation method of any one of claims 1 to 7;
the particle size of the artificial granite waste residue reinforced aggregate is 4-10mm.
9. The pervious concrete is characterized in that: the artificial granite waste residue reinforced aggregate comprises aggregate, cement, a water reducing agent and water, wherein the aggregate is the artificial granite waste residue reinforced aggregate in the claim 8.
10. The pervious concrete of claim 9, wherein: the mass ratio of the aggregate, the cement, the water reducing agent and the water is 1000-2000:500-600:1-2:100-200.
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