CN112876160B - Anchor rod grouting material for deep foundation pit construction and preparation method thereof - Google Patents
Anchor rod grouting material for deep foundation pit construction and preparation method thereof Download PDFInfo
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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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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/06—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyolefin as constituent
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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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
- C04B2111/70—Grouts, e.g. injection mixtures for cables for prestressed concrete
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Abstract
The invention discloses an anchor rod grouting material for deep foundation pit construction and a preparation method thereof, wherein an admixture, a part of an admixture and cement are uniformly mixed to obtain a solid material, then the other part of the admixture is added into water and uniformly stirred to obtain a premixed slurry, and finally the solid material is added into the premixed slurry and uniformly stirred to obtain the anchor rod grouting material; wherein the admixture is prepared by taking fly ash and corn straw powder as raw materials; the additive is prepared by modifying the aluminum silicate-calcium phosphate nanoparticles to obtain modified nanoparticles, performing polymerization reaction, adding the aluminum silicate-calcium phosphate nanoparticles in the polymerization process to obtain a polymer after the polymerization reaction is finished, mixing and heating the polymer and polypropylene to be molten, performing spinning to prepare fibers, and crushing. The obtained anchor rod grouting material has good flowability and high early strength, and the anchoring force is high after the anchor rod is grouted, so that the construction requirement of a deep foundation pit is met.
Description
Technical Field
The invention relates to a grouting material, in particular to an anchor rod grouting material for deep foundation pit construction and a preparation method thereof. Belongs to the technical field of building materials.
Background
With the continuous infiltration of urbanization process, deep foundation pit projects are increasing day by day, and soil nails and anchor rods are two most commonly used anchoring technologies in a temporary foundation pit supporting structure, and are widely applied to engineering construction of side slopes, foundation pit supports and the like due to high construction speed, safety, reliability, low construction difficulty and good economy.
According to investigation, the grouting material for the soil nails and the anchor rods in China is mainly ordinary portland cement, the water-cement mass ratio which is often adopted for ensuring the fluidity required by grouting operation is 0.5-0.55, the pure cement slurry liquid of the grouting mode has long setting time, the early strength of a solid body formed by grouting is low in engineering requirement, a maintenance period of more than seven days is usually needed after grouting is completed, the compressive strength of the grouting body can meet the engineering requirement, the construction period of the whole anchoring engineering is too long, and especially the grouting body is easy to lose efficacy in areas with high ground stress, deep parts or joint cracks, so that the instability of the whole supporting system can be caused.
Grouting materials have been developed rapidly, and the grouting materials used in actual construction at present can be systematically summarized into two main types, one is chemical grout, and the other is cement grout. The chemical grout not only has a series of advantages of good groutability, easy control of setting time, high stability, lower viscosity and the like, but also is easy to inject into tiny cracks in surrounding rocks. Commonly used chemical grouting materials include lignin, polyurethane, acrylamide, epoxy resin grout and novolac resins. However, chemical grouting has the disadvantages that the strength of the solid body formed by the injected slurry is not high and the slurry is easy to be polluted. In addition, chemical grout is relatively expensive compared to cement materials. The grouting material is rarely used in reinforcement engineering. The main types of the chemical grouting material are acid water glass slurry material, acrylate slurry material, rapidly solidified PBM concrete underwater, lignin slurry material and the like.
The other type of grouting material is cement grout, and the most widely used grouting material at present is pure cement neat grout. In addition, cement-clay mixed slurry, cement-fly ash mixed slurry and cement-water glass mixed double liquid are widely used. The cement grout has the advantages of wide raw material sources, low price and high strength of a formed consolidation body, and has the defects of long setting time, inaccurate control time, low stability, high water precipitation rate, low strength increase rate of the consolidation body, easy slurry leakage in a surrounding rock stratum with large pores, poor injectability in a surrounding rock stratum with microcracks, poor grouting quality and the like. The slurry material is applied and developed towards superfine cement, high water quick-setting material, silica powder cement slurry material and nano cement slurry material.
Generally speaking, the mobility of current stock slip casting material is relatively poor, and early strong is low to carry out the slip casting back anchoring force to the stock and hang down, can't satisfy deep basal pit construction requirement.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the anchor rod grouting material for deep foundation pit construction and the preparation method thereof, wherein the anchor rod grouting material has good fluidity, high early strength and high anchoring strength after anchor rod grouting, and meets the construction requirements of the deep foundation pit.
In order to achieve the purpose, the invention adopts the following technical scheme:
the preparation method of the anchor rod grouting material for the deep foundation pit construction comprises the following steps of firstly, uniformly mixing 30-40 parts by weight of admixture, 1-2 parts by weight of additive and 100 parts by weight of cement to obtain a solid material, then adding 2-3 parts by weight of additive into 55-65 parts by weight of water, uniformly stirring to obtain a premixed slurry, finally adding the solid material into the premixed slurry, and uniformly stirring to obtain the anchor rod grouting material; the admixture is prepared by adding water into fly ash and corn straw powder, uniformly stirring and mixing to prepare slurry with the solid content of 20-30 w.t%, and then performing microwave treatment, solid-liquid separation, drying, calcining and crushing; the additive is prepared by modifying aluminum silicate-calcium phosphate nanoparticles by using N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane to obtain modified nanoparticles, performing polymerization reaction by using acrylamide and N- (4-aminophenyl) acrylamide as raw materials, adding the aluminum silicate-calcium phosphate nanoparticles in the polymerization process, obtaining a polymer after the polymerization reaction is finished, mixing and heating the polymer and polypropylene until the polymer is molten, performing spinning to prepare fibers, and crushing.
Preferably, the cement is ordinary portland cement with the label P.052.5, the fly ash is second-grade fly ash, and the particle size of the corn straw powder is 100-150 meshes.
Preferably, when the admixture is prepared, the mass ratio of the fly ash to the corn stalk powder is 1: 0.2 to 0.3.
Preferably, when preparing the admixture, the process conditions of the microwave treatment are as follows: performing microwave treatment at 500-700W for 10-15 minutes; the calcination process conditions are as follows: calcining for 2-3 hours at 500-600 ℃.
Preferably, the admixture is crushed to a particle size of 100 to 150 mesh.
Preferably, the preparation method of the aluminum silicate-calcium phosphate nano particles comprises the following steps of: firstly, adding 3-5 parts of hexadecyl trimethyl ammonium bromide into 100 parts of water, uniformly stirring, simultaneously dropwise adding a calcium nitrate aqueous solution with the mass concentration of 15-20% and a disodium hydrogen phosphate aqueous solution with the mass concentration of 15-20% while stirring, carrying out a first stirring reaction to obtain a nano calcium phosphate suspension, controlling the temperature to be 35-45 ℃, adding cyclohexane into the nano calcium phosphate suspension, carrying out ultrasonic oscillation to obtain a mixed solution uniformly, then simultaneously dropwise adding the mixed solution and tetraethyl orthosilicate into a premixed solution containing aluminum nitrate and ammonia water, carrying out a second stirring reaction, and reacting the tetraethyl orthosilicate and the aluminum nitrate and depositing on the surface of nano calcium phosphate under the action of the ammonia water to obtain the aluminum silicate-calcium phosphate nanoparticles.
More preferably, the molar ratio of calcium nitrate contained in the calcium nitrate aqueous solution, disodium hydrogenphosphate contained in the disodium hydrogenphosphate aqueous solution, tetraethyl orthosilicate contained in the disodium hydrogenphosphate aqueous solution, and aluminum nitrate contained in the premix liquid is 1: 1: 1: 1, adding 1 part by weight of aluminum nitrate and 0.01 part by weight of ammonia water with the mass concentration of 22-25% into 5 parts by weight of water, and uniformly stirring to obtain the premixed solution.
Preferably, the dosage of the cyclohexane is 1-2 times of the weight of the nano calcium phosphate suspension, and the process conditions of the ultrasonic oscillation are as follows: ultrasonic oscillation at 400-600W for 40-50 minutes.
Further preferably, the calcium nitrate aqueous solution and the sodium silicate aqueous solution are slowly dripped at a constant speed for 30-40 minutes; and slowly dripping the mixed solution and tetraethyl orthosilicate at a constant speed for 5-6 hours.
Further preferably, the process conditions of the first stirring reaction are as follows: stirring and reacting for 5-7 hours at 50-60 ℃; the technological conditions of the second stirring reaction are as follows: and (4) keeping the temperature and stirring for reacting for 18-20 hours.
And preferably, after the second stirring reaction is finished, heating to 80-90 ℃ for demulsification, taking a water phase, and drying to obtain the aluminum silicate-calcium phosphate nano particles.
Preferably, the preparation method of the modified nanoparticles comprises the following steps in parts by weight: firstly, 1 part of N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane is dispersed in 5-7 parts of toluene by ultrasonic waves, then 0.4-0.6 part of aluminum silicate-calcium phosphate nanoparticles are added, the mixture is stirred and reacted for 6-8 hours at the temperature of 80-90 ℃, and the modified nanoparticles are obtained after centrifugation and drying.
Preferably, the preparation method of the polymer comprises the following steps in parts by weight: adding 1 part of acrylamide and 0.05-0.06 part of N- (4-aminophenyl) acrylamide into 3-5 parts of water, stirring until the acrylamide and the N- (4-aminophenyl) acrylamide are completely dissolved, transferring the mixture into a cobalt source chamber, irradiating the mixture for 3-4 hours at 68.34Gy/min, adding 0.5-0.6 part of modified nanoparticles, stirring and uniformly mixing the mixture, continuously irradiating the mixture for 6-8 hours at 108.93Gy/min to obtain hydrogel, and performing post-treatment to obtain the polymer.
Further preferably, the post-treatment method comprises the following specific steps: fully replacing water in the hydrogel by using normal hexane, drying by using carbon dioxide supercritical fluid to obtain dry gel, and crushing.
More preferably, the process conditions of the supercritical fluid drying by carbon dioxide are as follows: the pressure is 6-8 MPa, the temperature is 45-48 ℃, and the time is 7-9 hours.
Preferably, the mass ratio of polymer to polypropylene is 1: and 5-7, mixing and heating the two materials until the two materials are molten, dispersing the mixture for 2-3 hours at the melting temperature by using ultrasonic waves, then conveying the mixture to a spinning machine through a circulating pipeline, metering the mixture by using a metering pump, then feeding the mixture into a spinning nozzle through a filter and a connecting pipe, extruding the mixture through holes of the spinning nozzle to form a stock solution trickle with the pressure of 5-10 MPa, and finally obtaining the fiber through a coagulating bath.
More preferably, the solvent in the thin stream of the stock solution diffuses into the coagulation bath, and the coagulant in the coagulation bath permeates into the thin stream of the stock solution to reach a critical concentration, so that the fiber is precipitated in the coagulation bath, and the fiber is pulverized to 100 to 120 meshes.
Preferably, the coagulating bath is a water bath with the mass content of the coagulating agent of 5-10%, and the coagulating agent is CaCl2·2H2O, and MgCl2·H2O, the mass ratio of the two is 1: 2 to 3.
The anchor rod grouting material for deep foundation pit construction and the preparation method thereof are obtained by the preparation method.
The invention has the beneficial effects that:
firstly, uniformly mixing an admixture, a part of an admixture and cement to obtain a solid material, then adding the other part of the admixture into water, uniformly stirring to obtain a premixed slurry, finally adding the solid material into the premixed slurry, and uniformly stirring to obtain the anchor rod grouting material; the admixture is prepared by adding water into fly ash and corn straw powder, uniformly stirring and mixing to prepare slurry, and then performing microwave treatment, solid-liquid separation, drying, calcining and crushing; the additive is prepared by modifying aluminum silicate-calcium phosphate nanoparticles by using N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane to obtain modified nanoparticles, performing polymerization reaction by using acrylamide and N- (4-aminophenyl) acrylamide as raw materials, adding the aluminum silicate-calcium phosphate nanoparticles in the polymerization process, obtaining a polymer after the polymerization reaction is finished, mixing and heating the polymer and polypropylene until the polymer is molten, performing spinning to prepare fibers, and crushing. The obtained anchor rod grouting material has good flowability and high early strength, and the anchoring force is high after the anchor rod is grouted, so that the construction requirement of a deep foundation pit is met.
According to the invention, the admixture is separately fed, one part is added into the solid material, and the other part is pre-dispersed by water, so that the feeding is more beneficial to the contact of the admixture and cement, the fluidity is good, the growth direction of a cement hydration product is controlled, the early strength is effectively improved, and the anchoring force is higher after the anchor rod is grouted.
The admixture is prepared by taking fly ash and corn straw powder as raw materials, is subjected to microwave treatment and calcination treatment, has high activity, good compatibility with other components, improves the fluidity, further improves the early strength, and further improves the anchoring force after grouting the anchor rod.
The additive is prepared by feeding N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane modified aluminum silicate-calcium phosphate nanoparticles in the polymerization reaction process of acrylamide and N- (4-aminophenyl) acrylamide, wherein hydrogen bond action is formed between amino groups in the nanoparticles, pores have adsorption effect on other components, the fluidity and early strength are further improved, and the anchoring force is further enhanced after grouting the anchor rod. The polymer and the polypropylene are mixed to prepare fibers, thereby being beneficial to further improving the early strength and further improving the anchoring force after the anchor rod is grouted.
Detailed Description
The present invention will be further illustrated by the following examples, which are intended to be merely illustrative and not limitative.
Example 1:
the preparation method of the anchor rod grouting material for the deep foundation pit construction comprises the steps of firstly, uniformly mixing 30kg of admixture, 2kg of admixture and 100kg of cement to obtain a solid material, then adding 2kg of admixture into 65kg of water, uniformly stirring to obtain a premixed slurry, finally adding the solid material into the premixed slurry, and uniformly stirring to obtain the anchor rod grouting material; the admixture is prepared by adding water into fly ash and corn straw powder, uniformly stirring and mixing to prepare slurry with the solid content of 20 w.t%, and then performing microwave treatment, solid-liquid separation, drying, calcining and crushing; the additive is prepared by modifying aluminum silicate-calcium phosphate nanoparticles by using N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane to obtain modified nanoparticles, performing polymerization reaction by using acrylamide and N- (4-aminophenyl) acrylamide as raw materials, adding the aluminum silicate-calcium phosphate nanoparticles in the polymerization process, obtaining a polymer after the polymerization reaction is finished, mixing and heating the polymer and polypropylene until the polymer is molten, performing spinning to prepare fibers, and crushing.
The cement is ordinary portland cement with the label P.052.5, the fly ash is secondary fly ash, and the particle size of the corn straw powder is 150 meshes.
When preparing the admixture, the mass ratio of the fly ash to the corn straw powder is 1: 0.2.
when preparing the admixture, the process conditions of the microwave treatment are as follows: treating with 700W microwave for 10 minutes; the calcination process conditions are as follows: calcining at 600 ℃ for 2 hours.
The admixture was pulverized to a particle size of 150 mesh.
The preparation method of the aluminum silicate-calcium phosphate nano-particles comprises the following steps: firstly, adding 3kg of hexadecyl trimethyl ammonium bromide into 100kg of water, uniformly stirring, simultaneously dropwise adding a calcium nitrate aqueous solution with the mass concentration of 20% and a disodium hydrogen phosphate aqueous solution with the mass concentration of 15% while stirring, carrying out a first stirring reaction to obtain a nano calcium phosphate suspension, controlling the temperature to be 45 ℃, adding cyclohexane into the nano calcium phosphate suspension, carrying out ultrasonic oscillation to obtain a mixed solution uniformly, then simultaneously dropwise adding the mixed solution and tetraethyl orthosilicate into a premixed solution containing aluminum nitrate and ammonia water, carrying out a second stirring reaction, and reacting and depositing the tetraethyl orthosilicate and the aluminum nitrate on the surface of the nano calcium phosphate under the action of the ammonia water to obtain the aluminum silicate-calcium phosphate nanoparticles.
The molar ratio of calcium nitrate contained in the calcium nitrate aqueous solution, disodium hydrogen phosphate contained in the disodium hydrogen phosphate aqueous solution, tetraethyl orthosilicate contained in the disodium hydrogen phosphate aqueous solution and aluminum nitrate contained in the premix is 1: 1: 1: 1, adding 1kg of aluminum nitrate and 0.01kg of ammonia water with the mass concentration of 22% into 5kg of water, and uniformly stirring to obtain the premixed solution.
The dosage of cyclohexane is 2 times of the weight of the nano calcium phosphate suspension, and the process conditions of ultrasonic oscillation are as follows: the ultrasonic wave of 400W was oscillated for 50 minutes.
Slowly dripping the calcium nitrate aqueous solution and the sodium silicate aqueous solution at a constant speed for 30 minutes; the mixed solution and tetraethyl orthosilicate are slowly dripped at a constant speed for 6 hours.
The process conditions of the first stirring reaction are as follows: stirring and reacting for 7 hours at 50 ℃; the technological conditions of the second stirring reaction are as follows: the reaction was stirred for 18 hours with constant temperature.
Heating to 90 ℃ after the second stirring reaction is finished, demulsifying, taking the water phase, and drying to obtain the aluminum silicate-calcium phosphate nano particles.
The preparation method of the modified nano-particle comprises the following steps: firstly, 1kg of N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane is dispersed in 5kg of toluene by ultrasonic waves, then 0.6kg of aluminum silicate-calcium phosphate nano particles are added, stirred and reacted for 8 hours at the temperature of 80 ℃, centrifuged and dried, and the modified nano particles are obtained.
The preparation method of the polymer comprises the following steps: adding 1kg of acrylamide and 0.05kg of N- (4-aminophenyl) acrylamide into 5kg of water, stirring until the acrylamide and the acrylamide are completely dissolved, transferring the mixture into a cobalt source chamber, irradiating the mixture for 3 hours at 68.34Gy/min, adding 0.6kg of modified nanoparticles, stirring and uniformly mixing, continuously irradiating the mixture for 6 hours at 108.93Gy/min to obtain hydrogel, and performing post-treatment to obtain the polymer.
The specific method of post-treatment is as follows: fully replacing water in the hydrogel by using normal hexane, drying by using carbon dioxide supercritical fluid to obtain dry gel, and crushing.
The process conditions of the supercritical carbon dioxide fluid drying are as follows: the pressure is 8MPa, the temperature is 45 ℃, and the time is 9 hours.
The mass ratio of the polymer to the polypropylene is 1: and 5, mixing and heating the two materials to be molten, carrying out ultrasonic dispersion for 3 hours at the melting temperature, then conveying the mixture to a spinning machine through a circulating pipeline, metering the mixture by a metering pump, feeding the mixture into a spinning nozzle through a filter and a connecting pipe, extruding the mixture through holes of a spinneret plate to form a stock solution trickle with the pressure of 5MPa, and finally obtaining the fiber through a coagulating bath.
And (3) diffusing the solvent in the stock solution trickle to the coagulation bath, and permeating the coagulant in the coagulation bath to the stock solution trickle to ensure that the stock solution trickle reaches the critical concentration, precipitating in the coagulation bath to obtain fibers, and crushing to 120 meshes.
The coagulating bath is water bath with coagulator of 5 wt%, and the coagulator is CaCl2·2H2O, and MgCl2·H2O, and the mass ratio of the two is 1: 3.
example 2:
the preparation method of the anchor rod grouting material for the deep foundation pit construction comprises the steps of firstly uniformly mixing 40kg of admixture, 1kg of admixture and 100kg of cement to obtain a solid material, then adding 3kg of admixture into 55kg of water, uniformly stirring to obtain a premixed slurry, finally adding the solid material into the premixed slurry, and uniformly stirring to obtain the anchor rod grouting material; the admixture is prepared by adding water into fly ash and corn straw powder, uniformly stirring and mixing to prepare slurry with the solid content of 30 w.t%, and then performing microwave treatment, solid-liquid separation, drying, calcining and crushing; the additive is prepared by modifying aluminum silicate-calcium phosphate nanoparticles by using N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane to obtain modified nanoparticles, performing polymerization reaction by using acrylamide and N- (4-aminophenyl) acrylamide as raw materials, adding the aluminum silicate-calcium phosphate nanoparticles in the polymerization process, obtaining a polymer after the polymerization reaction is finished, mixing and heating the polymer and polypropylene until the polymer is molten, performing spinning to prepare fibers, and crushing.
The cement is ordinary portland cement with the label P.052.5, the fly ash is secondary fly ash, and the particle size of the corn straw powder is 100 meshes.
When preparing the admixture, the mass ratio of the fly ash to the corn straw powder is 1: 0.3.
when preparing the admixture, the process conditions of the microwave treatment are as follows: microwave treatment at 500W for 15 minutes; the calcination process conditions are as follows: calcining at 500 deg.C for 3 hr.
The admixture is crushed to a particle size of 100 mesh.
The preparation method of the aluminum silicate-calcium phosphate nano-particles comprises the following steps: firstly, adding 5kg of hexadecyl trimethyl ammonium bromide into 100kg of water, uniformly stirring, simultaneously dropwise adding a calcium nitrate aqueous solution with the mass concentration of 15% and a disodium hydrogen phosphate aqueous solution with the mass concentration of 20% while stirring, carrying out a first stirring reaction to obtain a nano calcium phosphate suspension, controlling the temperature to be 35 ℃, adding cyclohexane into the nano calcium phosphate suspension, carrying out ultrasonic oscillation to obtain a mixed solution uniformly, then simultaneously dropwise adding the mixed solution and tetraethyl orthosilicate into a premixed solution containing aluminum nitrate and ammonia water, carrying out a second stirring reaction, and reacting and depositing the tetraethyl orthosilicate and the aluminum nitrate on the surface of the nano calcium phosphate under the action of the ammonia water to obtain the aluminum silicate-calcium phosphate nanoparticles.
The molar ratio of calcium nitrate contained in the calcium nitrate aqueous solution, disodium hydrogen phosphate contained in the disodium hydrogen phosphate aqueous solution, tetraethyl orthosilicate contained in the disodium hydrogen phosphate aqueous solution and aluminum nitrate contained in the premix is 1: 1: 1: 1, adding 1kg of aluminum nitrate and 0.01kg of 25% ammonia water into 5kg of water, and uniformly stirring to obtain the premixed solution.
The dosage of cyclohexane is 1 time of the weight of the nano calcium phosphate suspension, and the process conditions of ultrasonic oscillation are as follows: ultrasonic oscillation at 600W for 40 minutes.
Slowly dripping the calcium nitrate aqueous solution and the sodium silicate aqueous solution at a constant speed for 40 minutes; the mixed solution and tetraethyl orthosilicate are slowly dripped at a constant speed for 5 hours.
The process conditions of the first stirring reaction are as follows: stirring and reacting for 5 hours at the temperature of 60 ℃; the process conditions of the second stirring reaction are as follows: the reaction was stirred for 20 hours with heat preservation.
Heating to 80 ℃ after the second stirring reaction is finished, demulsifying, taking the water phase, and drying to obtain the aluminum silicate-calcium phosphate nano particles.
The preparation method of the modified nano-particle comprises the following steps: firstly, 1kg of N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane is dispersed in 7kg of toluene by ultrasonic waves, then 0.4kg of aluminum silicate-calcium phosphate nano particles are added, stirred and reacted for 6 hours at 90 ℃, centrifuged and dried, and the modified nano particles are obtained.
The preparation method of the polymer comprises the following steps: adding 1kg of acrylamide and 0.06kg of N- (4-aminophenyl) acrylamide into 3kg of water, stirring until the acrylamide and the 4kg of N- (4-aminophenyl) acrylamide are completely dissolved, transferring the mixture into a cobalt source chamber, irradiating the mixture for 4 hours at 68.34Gy/min, adding 0.5kg of modified nanoparticles, stirring and uniformly mixing the mixture, continuously irradiating the mixture for 8 hours at 108.93Gy/min to obtain hydrogel, and performing post-treatment to obtain the polymer.
The specific method of post-treatment is as follows: fully replacing water in the hydrogel by using normal hexane, drying by using carbon dioxide supercritical fluid to obtain dry gel, and crushing.
The process conditions of the supercritical carbon dioxide fluid drying are as follows: the pressure is 6MPa, the temperature is 48 ℃, and the time is 7 hours.
The mass ratio of the polymer to the polypropylene is 1: and 7, mixing and heating the two materials to be molten, carrying out ultrasonic dispersion for 2 hours at the melting temperature, then sending the mixture to a spinning machine through a circulating pipeline, metering the mixture through a metering pump, then entering a spinning nozzle through a filter and a connecting pipe, extruding the mixture through holes of a spinneret plate to form a stock solution trickle with the pressure of 10MPa, and finally obtaining the fiber through a coagulating bath.
And (3) diffusing the solvent in the stock solution trickle to the coagulation bath, and permeating the coagulant in the coagulation bath to the stock solution trickle to ensure that the stock solution trickle reaches the critical concentration, precipitating in the coagulation bath to obtain fibers, and crushing to 100 meshes.
The coagulating bath is water bath with 10% mass content of coagulating agent, and the coagulating agent is CaCl2·2H2O, and MgCl2·H2O, the mass ratio of the two is 1: 2.
example 3:
firstly, uniformly mixing 35kg of admixture, 1.5kg of additive and 100kg of cement to obtain a solid material, then adding 2.5kg of additive into 60kg of water, uniformly stirring to obtain a premixed slurry, finally adding the solid material into the premixed slurry, and uniformly stirring to obtain the anchor rod grouting material; the admixture is prepared by adding water into fly ash and corn straw powder, uniformly stirring and mixing to prepare slurry with the solid content of 25 w.t%, and then performing microwave treatment, solid-liquid separation, drying, calcining and crushing; the additive is prepared by modifying aluminum silicate-calcium phosphate nanoparticles by using N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane to obtain modified nanoparticles, performing polymerization reaction by using acrylamide and N- (4-aminophenyl) acrylamide as raw materials, adding the aluminum silicate-calcium phosphate nanoparticles in the polymerization process, obtaining a polymer after the polymerization reaction is finished, mixing and heating the polymer and polypropylene until the polymer is molten, performing spinning to prepare fibers, and crushing.
The cement is ordinary portland cement with the label P.052.5, the fly ash is secondary fly ash, and the particle size of the corn straw powder is 120 meshes.
When preparing the admixture, the mass ratio of the fly ash to the corn straw powder is 1: 0.25.
when preparing the admixture, the process conditions of the microwave treatment are as follows: microwave treatment at 600W for 12 minutes; the calcination process conditions are as follows: calcining at 550 ℃ for 2.5 hours.
The admixture is crushed to 120 mesh.
The preparation method of the aluminum silicate-calcium phosphate nano-particles comprises the following steps: firstly, adding 4kg of hexadecyl trimethyl ammonium bromide into 100kg of water, uniformly stirring, simultaneously dropwise adding a calcium nitrate aqueous solution with the mass concentration of 18% and a disodium hydrogen phosphate aqueous solution with the mass concentration of 18% while stirring, carrying out a first stirring reaction to obtain a nano calcium phosphate suspension, controlling the temperature to be 40 ℃, adding cyclohexane into the nano calcium phosphate suspension, carrying out ultrasonic oscillation to obtain a mixed solution uniformly, then simultaneously dropwise adding the mixed solution and tetraethyl orthosilicate into a premixed solution containing aluminum nitrate and ammonia water, carrying out a second stirring reaction, and reacting and depositing the tetraethyl orthosilicate and the aluminum nitrate on the surface of the nano calcium phosphate under the action of the ammonia water to obtain the aluminum silicate-calcium phosphate nanoparticles.
The molar ratio of calcium nitrate contained in the calcium nitrate aqueous solution, disodium hydrogen phosphate contained in the disodium hydrogen phosphate aqueous solution, tetraethyl orthosilicate contained in the disodium hydrogen phosphate aqueous solution and aluminum nitrate contained in the premix is 1: 1: 1: 1, adding 1kg of aluminum nitrate and 0.01kg of 23% ammonia water into 5kg of water, and uniformly stirring to obtain the premixed solution.
The dosage of the cyclohexane is 1.5 times of the weight of the nano calcium phosphate suspension, and the process conditions of the ultrasonic oscillation are as follows: 500W ultrasonic vibration was carried out for 45 minutes.
Slowly dripping the calcium nitrate aqueous solution and the sodium silicate aqueous solution at a constant speed for 35 minutes; the mixed solution and tetraethyl orthosilicate are slowly dripped at a constant speed for 5.5 hours.
The process conditions of the first stirring reaction are as follows: stirring and reacting for 6 hours at 55 ℃; the technological conditions of the second stirring reaction are as follows: the reaction was stirred for 16 hours with heat preservation.
Heating to 85 ℃ for demulsification after the second stirring reaction is finished, taking the water phase, and drying to obtain the aluminum silicate-calcium phosphate nano particles.
The preparation method of the modified nano-particle comprises the following steps: firstly, 1kg of N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane is dispersed in 6kg of toluene by ultrasonic waves, then 0.5kg of aluminum silicate-calcium phosphate nano particles are added, the mixture is stirred and reacted for 7 hours at 85 ℃, and the mixture is centrifuged and dried to obtain the modified nano particles.
The preparation method of the polymer comprises the following steps: adding 1kg of acrylamide and 0.055kg of N- (4-aminophenyl) acrylamide into 4kg of water, stirring until the acrylamide and the water are completely dissolved, transferring the mixture into a cobalt source chamber, irradiating the mixture for 3.5 hours at 68.34Gy/min, adding 0.55kg of modified nanoparticles, stirring and uniformly mixing the mixture, continuously irradiating the mixture for 7 hours at 108.93Gy/min to obtain hydrogel, and performing post-treatment to obtain the polymer.
The specific method of post-treatment is as follows: fully replacing water in the hydrogel by using normal hexane, drying by using carbon dioxide supercritical fluid to obtain dry gel, and crushing.
The process conditions of the supercritical carbon dioxide fluid drying are as follows: the pressure is 7MPa, the temperature is 47 ℃, and the time is 8 hours.
The mass ratio of the polymer to the polypropylene is 1: and 6, mixing and heating the two materials to be molten, carrying out ultrasonic dispersion for 2.5 hours at the melting temperature, then sending the mixture to a spinning machine through a circulating pipeline, metering the mixture through a metering pump, then entering a spinning nozzle through a filter and a connecting pipe, extruding the mixture through holes of a spinneret plate to form a stock solution trickle with the pressure of 8MPa, and finally obtaining the fiber through a coagulating bath.
And (3) diffusing the solvent in the stock solution trickle to a coagulation bath, and permeating a coagulant in the coagulation bath into the stock solution trickle to ensure that the stock solution trickle reaches a critical concentration, precipitating in the coagulation bath to obtain fibers, and crushing to 110 meshes.
The coagulating bath is water bath with 8% mass content of coagulating agent, and the coagulating agent is CaCl2·2H2O, and MgCl2·H2O, the mass ratio of the two is 1: 2.5.
comparative example 1
A preparation method of an anchor rod grouting material for deep foundation pit construction comprises the steps of directly adding 30kg of admixture, 4kg of admixture and 100kg of cement into 65kg of water, and uniformly stirring to obtain the anchor rod grouting material; the admixture is prepared by adding water into fly ash and corn straw powder, uniformly stirring and mixing to prepare slurry with the solid content of 20 w.t%, and then performing microwave treatment, solid-liquid separation, drying, calcining and crushing; the additive is prepared by modifying aluminum silicate-calcium phosphate nano particles by using N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane to obtain modified nano particles, then performing polymerization reaction by using acrylamide and N- (4-aminophenyl) acrylamide as raw materials, adding the aluminum silicate-calcium phosphate nano particles in the polymerization process to obtain a polymer after the polymerization reaction is finished, then mixing and heating the polymer and polypropylene until the polymer is molten, performing spinning to prepare fibers, and crushing the fibers.
The cement is ordinary portland cement with the label P.052.5, the fly ash is secondary fly ash, and the particle size of the corn straw powder is 150 meshes.
When preparing the admixture, the mass ratio of the fly ash to the corn straw powder is 1: 0.2.
when preparing the admixture, the process conditions of the microwave treatment are as follows: treating with 700W microwave for 10 minutes; the calcining process conditions are as follows: calcining at 600 ℃ for 2 hours.
The admixture is crushed to a particle size of 150 mesh.
The preparation method of the aluminum silicate-calcium phosphate nano-particles comprises the following steps: firstly, adding 3kg of hexadecyl trimethyl ammonium bromide into 100kg of water, uniformly stirring, simultaneously dropwise adding a calcium nitrate aqueous solution with the mass concentration of 20% and a disodium hydrogen phosphate aqueous solution with the mass concentration of 15% while stirring, carrying out a first stirring reaction to obtain a nano calcium phosphate suspension, controlling the temperature to be 45 ℃, adding cyclohexane into the nano calcium phosphate suspension, carrying out ultrasonic oscillation to obtain a mixed solution uniformly, then simultaneously dropwise adding the mixed solution and tetraethyl orthosilicate into a premixed solution containing aluminum nitrate and ammonia water, carrying out a second stirring reaction, and reacting and depositing the tetraethyl orthosilicate and the aluminum nitrate on the surface of the nano calcium phosphate under the action of the ammonia water to obtain the aluminum silicate-calcium phosphate nanoparticles.
The molar ratio of calcium nitrate contained in the calcium nitrate aqueous solution, disodium hydrogen phosphate contained in the disodium hydrogen phosphate aqueous solution, tetraethyl orthosilicate contained in the disodium hydrogen phosphate aqueous solution and aluminum nitrate contained in the premix is 1: 1: 1: 1, adding 1kg of aluminum nitrate and 0.01kg of ammonia water with the mass concentration of 22% into 5kg of water, and uniformly stirring to obtain the premixed solution.
The dosage of cyclohexane is 2 times of the weight of the nano calcium phosphate suspension, and the process conditions of ultrasonic oscillation are as follows: the ultrasonic wave of 400W was oscillated for 50 minutes.
Slowly dripping the calcium nitrate aqueous solution and the sodium silicate aqueous solution at a constant speed for 30 minutes; the mixed solution and tetraethyl orthosilicate are slowly dripped at a constant speed for 6 hours.
The process conditions of the first stirring reaction are as follows: stirring and reacting for 7 hours at 50 ℃; the technological conditions of the second stirring reaction are as follows: the reaction was stirred for 18 hours with constant temperature.
Heating to 90 ℃ after the second stirring reaction is finished, demulsifying, taking the water phase, and drying to obtain the aluminum silicate-calcium phosphate nano particles.
The preparation method of the modified nano-particle comprises the following steps: firstly, 1kg of N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane is dispersed in 5kg of toluene by ultrasonic waves, then 0.6kg of aluminum silicate-calcium phosphate nano particles are added, stirred and reacted for 8 hours at the temperature of 80 ℃, centrifuged and dried, and the modified nano particles are obtained.
The preparation method of the polymer comprises the following steps: adding 1kg of acrylamide and 0.05kg of N- (4-aminophenyl) acrylamide into 5kg of water, stirring until the acrylamide and the acrylamide are completely dissolved, transferring the mixture into a cobalt source chamber, irradiating the mixture for 3 hours at 68.34Gy/min, adding 0.6kg of modified nanoparticles, stirring and uniformly mixing, continuously irradiating the mixture for 6 hours at 108.93Gy/min to obtain hydrogel, and performing post-treatment to obtain the polymer.
The specific method of post-treatment is as follows: fully replacing water in the hydrogel by using normal hexane, drying by using carbon dioxide supercritical fluid to obtain dry gel, and crushing.
The process conditions of the supercritical carbon dioxide fluid drying are as follows: the pressure is 8MPa, the temperature is 45 ℃, and the time is 9 hours.
The mass ratio of the polymer to the polypropylene is 1: and 5, mixing and heating the two materials to be molten, carrying out ultrasonic dispersion for 3 hours at the melting temperature, then conveying the mixture to a spinning machine through a circulating pipeline, metering the mixture by a metering pump, feeding the mixture into a spinning nozzle through a filter and a connecting pipe, extruding the mixture through holes of a spinneret plate to form a stock solution trickle with the pressure of 5MPa, and finally obtaining the fiber through a coagulating bath.
And (3) diffusing the solvent in the stock solution trickle to the coagulation bath, and permeating the coagulant in the coagulation bath to the stock solution trickle to ensure that the stock solution trickle reaches the critical concentration, precipitating in the coagulation bath to obtain fibers, and crushing to 120 meshes.
The coagulating bath is water bath with coagulator of 5 wt%, and the coagulator is CaCl2·2H2O, and MgCl2·H2O, the mass ratio of the two is 1: 3.
comparative example 2
The preparation method of the anchor rod grouting material for the deep foundation pit construction comprises the steps of firstly, uniformly mixing 30kg of admixture, 2kg of admixture and 100kg of cement to obtain a solid material, then adding 2kg of admixture into 65kg of water, uniformly stirring to obtain a premixed slurry, finally adding the solid material into the premixed slurry, and uniformly stirring to obtain the anchor rod grouting material; the admixture is prepared by adding water into the fly ash, uniformly stirring and mixing the fly ash and the water to prepare slurry with the solid content of 20 w.t%, performing microwave treatment, performing solid-liquid separation, drying, calcining and crushing; the additive is prepared by modifying aluminum silicate-calcium phosphate nanoparticles by using N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane to obtain modified nanoparticles, performing polymerization reaction by using acrylamide and N- (4-aminophenyl) acrylamide as raw materials, adding the aluminum silicate-calcium phosphate nanoparticles in the polymerization process, obtaining a polymer after the polymerization reaction is finished, mixing and heating the polymer and polypropylene until the polymer is molten, performing spinning to prepare fibers, and crushing.
The cement is ordinary portland cement with the label P.052.5, and the fly ash is secondary fly ash.
When preparing the admixture, the process conditions of the microwave treatment are as follows: treating with 700W microwave for 10 minutes; the calcination process conditions are as follows: calcining at 600 ℃ for 2 hours.
The admixture is crushed to a particle size of 150 mesh.
The preparation method of the aluminum silicate-calcium phosphate nano-particles comprises the following steps: firstly, adding 3kg of hexadecyl trimethyl ammonium bromide into 100kg of water, uniformly stirring, simultaneously dropwise adding a calcium nitrate aqueous solution with the mass concentration of 20% and a disodium hydrogen phosphate aqueous solution with the mass concentration of 15% while stirring, carrying out a first stirring reaction to obtain a nano calcium phosphate suspension, controlling the temperature to be 45 ℃, adding cyclohexane into the nano calcium phosphate suspension, carrying out ultrasonic oscillation to obtain a mixed solution uniformly, then simultaneously dropwise adding the mixed solution and tetraethyl orthosilicate into a premixed solution containing aluminum nitrate and ammonia water, carrying out a second stirring reaction, and reacting and depositing the tetraethyl orthosilicate and the aluminum nitrate on the surface of the nano calcium phosphate under the action of the ammonia water to obtain the aluminum silicate-calcium phosphate nanoparticles.
The molar ratio of calcium nitrate contained in the calcium nitrate aqueous solution, disodium hydrogen phosphate contained in the disodium hydrogen phosphate aqueous solution, tetraethyl orthosilicate contained in the disodium hydrogen phosphate aqueous solution and aluminum nitrate contained in the premix is 1: 1: 1: 1, adding 1kg of aluminum nitrate and 0.01kg of ammonia water with the mass concentration of 22% into 5kg of water, and uniformly stirring to obtain the premixed solution.
The dosage of cyclohexane is 2 times of the weight of the nano calcium phosphate suspension, and the process conditions of ultrasonic oscillation are as follows: the ultrasonic wave of 400W was oscillated for 50 minutes.
Slowly dripping the calcium nitrate aqueous solution and the sodium silicate aqueous solution at a constant speed for 30 minutes; the mixed solution and tetraethyl orthosilicate are slowly dripped at a constant speed for 6 hours.
The process conditions of the first stirring reaction are as follows: stirring and reacting for 7 hours at 50 ℃; the technological conditions of the second stirring reaction are as follows: the reaction was stirred for 18 hours with constant temperature.
Heating to 90 ℃ after the second stirring reaction is finished, demulsifying, taking the water phase, and drying to obtain the aluminum silicate-calcium phosphate nano particles.
The preparation method of the modified nano-particle comprises the following steps: firstly, 1kg of N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane is dispersed in 5kg of toluene by ultrasonic waves, then 0.6kg of aluminum silicate-calcium phosphate nano particles are added, stirred and reacted for 8 hours at the temperature of 80 ℃, centrifuged and dried, and the modified nano particles are obtained.
The preparation method of the polymer comprises the following steps: adding 1kg of acrylamide and 0.05kg of N- (4-aminophenyl) acrylamide into 5kg of water, stirring until the acrylamide and the acrylamide are completely dissolved, transferring the mixture into a cobalt source chamber, irradiating the mixture for 3 hours at 68.34Gy/min, adding 0.6kg of modified nanoparticles, stirring and uniformly mixing, continuously irradiating the mixture for 6 hours at 108.93Gy/min to obtain hydrogel, and performing post-treatment to obtain the polymer.
The specific method of post-treatment is as follows: fully replacing water in the hydrogel by using normal hexane, drying by using carbon dioxide supercritical fluid to obtain dry gel, and crushing.
The process conditions of the supercritical carbon dioxide fluid drying are as follows: the pressure is 8MPa, the temperature is 45 ℃, and the time is 9 hours.
The mass ratio of the polymer to the polypropylene is 1: and 5, mixing and heating the two materials to be molten, carrying out ultrasonic dispersion for 3 hours at the melting temperature, then conveying the mixture to a spinning machine through a circulating pipeline, metering the mixture by a metering pump, feeding the mixture into a spinning nozzle through a filter and a connecting pipe, extruding the mixture through holes of a spinneret plate to form a stock solution trickle with the pressure of 5MPa, and finally obtaining the fiber through a coagulating bath.
And (3) diffusing the solvent in the stock solution trickle to the coagulation bath, and permeating the coagulant in the coagulation bath to the stock solution trickle to ensure that the stock solution trickle reaches the critical concentration, precipitating in the coagulation bath to obtain fibers, and crushing to 120 meshes.
The coagulating bath is water bath with coagulator of 5 wt%, and the coagulator is CaCl2·2H2O, and MgCl2·H2O, the mass ratio of the two is 1: 3.
comparative example 3
The preparation method of the anchor rod grouting material for the deep foundation pit construction comprises the steps of firstly, uniformly mixing 30kg of admixture, 2kg of admixture and 100kg of cement to obtain a solid material, then adding 2kg of admixture into 65kg of water, uniformly stirring to obtain a premixed slurry, finally adding the solid material into the premixed slurry, and uniformly stirring to obtain the anchor rod grouting material; the admixture is prepared by adding water into fly ash and corn straw powder, uniformly stirring and mixing to prepare slurry with the solid content of 20 w.t%, and then performing microwave treatment, solid-liquid separation, drying, calcining and crushing; the additive is prepared by modifying calcium phosphate nanoparticles with N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane to obtain modified nanoparticles, polymerizing acrylamide and N- (4-aminophenyl) acrylamide, adding aluminum silicate-calcium phosphate nanoparticles during polymerization to obtain polymer, mixing the polymer with polypropylene, heating to melt, spinning to obtain fibers, and pulverizing.
The cement is ordinary portland cement with the label P.052.5, the fly ash is secondary fly ash, and the particle size of the corn straw powder is 150 meshes.
When preparing the admixture, the mass ratio of the fly ash to the corn straw powder is 1: 0.2.
when preparing the admixture, the process conditions of the microwave treatment are as follows: treating with 700W microwave for 10 minutes; the calcination process conditions are as follows: calcining at 600 ℃ for 2 hours.
The admixture is crushed to a particle size of 150 mesh.
The preparation method of the calcium phosphate nano-particles comprises the following steps: firstly, adding 3kg of hexadecyl trimethyl ammonium bromide into 100kg of water, uniformly stirring, simultaneously dropwise adding a calcium nitrate aqueous solution with the mass concentration of 20% and a disodium hydrogen phosphate aqueous solution with the mass concentration of 15% while stirring, stirring for reaction, and carrying out post-treatment to obtain the calcium phosphate nano particles.
The molar ratio of calcium nitrate contained in the calcium nitrate aqueous solution to disodium hydrogen phosphate contained in the disodium hydrogen phosphate aqueous solution is 1: 1.
slowly dripping the calcium nitrate aqueous solution and the sodium silicate aqueous solution at a constant speed for 30 minutes.
The technological conditions of the stirring reaction are as follows: the reaction was stirred at 50 ℃ for 7 hours.
The specific method of post-treatment is as follows: heating to 90 deg.C for demulsification, collecting water phase, and drying to obtain calcium phosphate nanoparticles.
The preparation method of the modified nano-particle comprises the following steps: firstly, 1kg of N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane is dispersed in 5kg of toluene by ultrasonic waves, then 0.6kg of calcium phosphate nanoparticles are added, stirred and reacted for 8 hours at 80 ℃, centrifuged and dried, and the modified nanoparticles are obtained.
The polymer was prepared as follows: adding 1kg of acrylamide and 0.05kg of N- (4-aminophenyl) acrylamide into 5kg of water, stirring until the acrylamide and the acrylamide are completely dissolved, transferring the mixture into a cobalt source chamber, irradiating the mixture for 3 hours at 68.34Gy/min, adding 0.6kg of modified nanoparticles, stirring and uniformly mixing, continuously irradiating the mixture for 6 hours at 108.93Gy/min to obtain hydrogel, and performing post-treatment to obtain the polymer.
The specific method of post-treatment is as follows: fully replacing water in the hydrogel by using normal hexane, drying by using carbon dioxide supercritical fluid to obtain dry gel, and crushing.
The process conditions of the supercritical carbon dioxide fluid drying are as follows: the pressure is 8MPa, the temperature is 45 ℃, and the time is 9 hours.
The mass ratio of the polymer to the polypropylene is 1: and 5, mixing and heating the two materials to be molten, carrying out ultrasonic dispersion for 3 hours at the melting temperature, then conveying the mixture to a spinning machine through a circulating pipeline, metering the mixture by a metering pump, feeding the mixture into a spinning nozzle through a filter and a connecting pipe, extruding the mixture through holes of a spinneret plate to form a stock solution trickle with the pressure of 5MPa, and finally obtaining the fiber through a coagulating bath.
And (3) diffusing the solvent in the stock solution trickle to the coagulation bath, and permeating the coagulant in the coagulation bath to the stock solution trickle to ensure that the stock solution trickle reaches the critical concentration, precipitating in the coagulation bath to obtain fibers, and crushing to 120 meshes.
The coagulating bath is water bath with coagulator of 5 wt%, and the coagulator is CaCl2·2H2O, and MgCl2·H2O, the mass ratio of the two is 1: 3.
comparative example 4
The preparation method of the anchor rod grouting material for the deep foundation pit construction comprises the steps of firstly, uniformly mixing 30kg of admixture, 2kg of admixture and 100kg of cement to obtain a solid material, then adding 2kg of admixture into 65kg of water, uniformly stirring to obtain a premixed slurry, finally adding the solid material into the premixed slurry, and uniformly stirring to obtain the anchor rod grouting material; the admixture is prepared by adding water into fly ash and corn straw powder, uniformly stirring and mixing to prepare slurry with the solid content of 20 w.t%, and then performing microwave treatment, solid-liquid separation, drying, calcining and crushing; the additive is prepared by modifying aluminum silicate-calcium phosphate nanoparticles by using N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane to obtain modified nanoparticles, performing polymerization reaction by using acrylamide and N- (4-aminophenyl) acrylamide as raw materials, adding the aluminum silicate-calcium phosphate nanoparticles in the polymerization process, obtaining a polymer after the polymerization reaction is finished, and crushing the polymer to 120 meshes.
The cement is ordinary portland cement with the label P.052.5, the fly ash is secondary fly ash, and the particle size of the corn straw powder is 150 meshes.
When preparing the admixture, the mass ratio of the fly ash to the corn straw powder is 1: 0.2.
when preparing the admixture, the process conditions of the microwave treatment are as follows: treating with 700W microwave for 10 minutes; the calcination process conditions are as follows: calcining at 600 ℃ for 2 hours.
The admixture is crushed to a particle size of 150 mesh.
The preparation method of the aluminum silicate-calcium phosphate nano-particles comprises the following steps: firstly, adding 3kg of hexadecyl trimethyl ammonium bromide into 100kg of water, uniformly stirring, simultaneously dropwise adding a calcium nitrate aqueous solution with the mass concentration of 20% and a disodium hydrogen phosphate aqueous solution with the mass concentration of 15% while stirring, carrying out a first stirring reaction to obtain a nano calcium phosphate suspension, controlling the temperature to be 45 ℃, adding cyclohexane into the nano calcium phosphate suspension, carrying out ultrasonic oscillation to obtain a mixed solution uniformly, then simultaneously dropwise adding the mixed solution and tetraethyl orthosilicate into a premixed solution containing aluminum nitrate and ammonia water, carrying out a second stirring reaction, and reacting and depositing the tetraethyl orthosilicate and the aluminum nitrate on the surface of the nano calcium phosphate under the action of the ammonia water to obtain the aluminum silicate-calcium phosphate nanoparticles.
The molar ratio of calcium nitrate contained in the calcium nitrate aqueous solution, disodium hydrogen phosphate contained in the disodium hydrogen phosphate aqueous solution, tetraethyl orthosilicate contained in the disodium hydrogen phosphate aqueous solution and aluminum nitrate contained in the premix is 1: 1: 1: 1, adding 1kg of aluminum nitrate and 0.01kg of ammonia water with the mass concentration of 22% into 5kg of water, and uniformly stirring to obtain the premixed solution.
The dosage of cyclohexane is 2 times of the weight of the nano calcium phosphate suspension, and the process conditions of ultrasonic oscillation are as follows: the ultrasonic wave of 400W was oscillated for 50 minutes.
Slowly dripping the calcium nitrate aqueous solution and the sodium silicate aqueous solution at a constant speed for 30 minutes; the mixed solution and tetraethyl orthosilicate are slowly dripped at a constant speed for 6 hours.
The process conditions of the first stirring reaction are as follows: stirring and reacting for 7 hours at 50 ℃; the technological conditions of the second stirring reaction are as follows: the reaction was stirred for 18 hours with constant temperature.
Heating to 90 ℃ after the second stirring reaction is finished, demulsifying, taking a water phase, and drying to obtain the aluminum silicate-calcium phosphate nano particles.
The preparation method of the modified nano-particle comprises the following steps: firstly, 1kg of N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane is dispersed in 5kg of toluene by ultrasonic waves, then 0.6kg of aluminum silicate-calcium phosphate nano particles are added, stirred and reacted for 8 hours at the temperature of 80 ℃, centrifuged and dried, and the modified nano particles are obtained.
The preparation method of the polymer comprises the following steps: adding 1kg of acrylamide and 0.05kg of N- (4-aminophenyl) acrylamide into 5kg of water, stirring until the acrylamide and the acrylamide are completely dissolved, transferring the mixture into a cobalt source chamber, irradiating the mixture for 3 hours at 68.34Gy/min, adding 0.6kg of modified nanoparticles, stirring and uniformly mixing, continuously irradiating the mixture for 6 hours at 108.93Gy/min to obtain hydrogel, and performing post-treatment to obtain the polymer.
The specific method of post-treatment is as follows: fully replacing water in the hydrogel by using normal hexane, drying by using carbon dioxide supercritical fluid to obtain dry gel, and crushing.
The process conditions of the supercritical carbon dioxide fluid drying are as follows: the pressure is 8MPa, the temperature is 45 ℃, and the time is 9 hours.
Test examples
The performance of the grouting materials obtained in examples 1 to 3 and comparative examples 1 to 4 was examined, and the results are shown in Table 1.
Wherein, the fluidity is referred to TB/T3192-2008 (detected at the temperature of 20 ℃ in a standard laboratory), and the compressive strength is referred to GB/T17671.
And (4) carrying out grouting and drawing tests on the anchor rod of the deep foundation pit (the diameter of the anchor rod is 76mm), and testing the anchoring force.
TABLE 1 Performance test results
As can be seen from Table 1, the grouting materials obtained in examples 1 to 3 have good flowability, good early strength and large anchor rod anchoring force after grouting.
The direct mixing method is adopted in the comparative example 1, the corn straw powder is omitted in the comparative example 2 when the admixture is prepared, the calcium phosphate nano-ions are used for replacing the aluminum silicate-calcium phosphate nano-particles in the comparative example 3 when the admixture is prepared, the step of spinning and fiber making is omitted in the comparative example 4 when the admixture is prepared, the flowability and the early strength of the obtained anchor rod grouting material are poor, and the anchoring force after grouting is also obviously poor, so that the components and the feeding method of the invention synergistically improve various performance indexes.
Although the present invention has been described with reference to the specific embodiments, it is not intended to limit the scope of the present invention, and various modifications and variations can be made by those skilled in the art without inventive changes based on the technical solution of the present invention.
Claims (6)
1. The preparation method of the anchor rod grouting material for deep foundation pit construction is characterized by comprising the following steps of firstly, uniformly mixing 30-40 parts by weight of admixture, 1-2 parts by weight of additive and 100 parts by weight of cement to obtain a solid material, then adding 2-3 parts by weight of additive into 55-65 parts by weight of water, uniformly stirring to obtain a premixed slurry, finally adding the solid material into the premixed slurry, and uniformly stirring to obtain the anchor rod grouting material; the admixture is prepared by adding water into fly ash and corn straw powder, uniformly stirring and mixing to prepare slurry with the solid content of 20-30 wt%, and then performing microwave treatment, solid-liquid separation, drying, calcining and crushing; the additive is prepared by modifying aluminum silicate-calcium phosphate nanoparticles by using N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane to obtain modified nanoparticles, then performing polymerization reaction by using acrylamide and N- (4-aminophenyl) acrylamide as raw materials, adding the modified aluminum silicate-calcium phosphate nanoparticles in the polymerization process, performing post-treatment after the polymerization reaction is finished to obtain a polymer, then mixing and heating the polymer and polypropylene to be molten, performing spinning to prepare fibers, and crushing;
the preparation method of the aluminum silicate-calcium phosphate nano-particles comprises the following steps of: firstly, adding 3-5 parts of hexadecyl trimethyl ammonium bromide into 100 parts of water, uniformly stirring, simultaneously dropwise adding a calcium nitrate aqueous solution with the mass concentration of 15-20% and a disodium hydrogen phosphate aqueous solution with the mass concentration of 15-20% while stirring, carrying out a first stirring reaction to obtain a nano calcium phosphate suspension, controlling the temperature to be 35-45 ℃, adding cyclohexane into the nano calcium phosphate suspension, carrying out ultrasonic oscillation to obtain a mixed solution uniformly, then simultaneously dropwise adding the mixed solution and tetraethyl orthosilicate into a premixed solution containing aluminum nitrate and ammonia water, carrying out a second stirring reaction, and reacting the tetraethyl orthosilicate and the aluminum nitrate and depositing on the surface of nano calcium phosphate under the action of the ammonia water to obtain aluminum silicate-calcium phosphate nanoparticles;
the preparation method of the polymer comprises the following steps of: adding 1 part of acrylamide and 0.05-0.06 part of N- (4-aminophenyl) acrylamide into 3-5 parts of water, stirring until the acrylamide and the N- (4-aminophenyl) acrylamide are completely dissolved, transferring the mixture into a cobalt source chamber, irradiating the mixture for 3-4 hours at 68.34Gy/min, adding 0.5-0.6 part of modified nanoparticles, stirring and uniformly mixing the mixture, continuously irradiating the mixture for 6-8 hours at 108.93Gy/min to obtain hydrogel, and performing post-treatment to obtain the polymer; the post-treatment method comprises the following specific steps: fully replacing water in the hydrogel by using normal hexane, drying by using carbon dioxide supercritical fluid to obtain dry gel, and crushing.
2. The preparation method of claim 1, wherein the cement is Portland cement with the reference number P.052.5, the fly ash is second-grade fly ash, and the particle size of the corn straw powder is 100-150 meshes.
3. The preparation method of claim 1, wherein the mass ratio of the fly ash to the corn stalk powder is 1: 0.2 to 0.3.
4. The preparation method according to claim 1, wherein the process conditions of the microwave treatment in preparing the admixture are as follows: performing microwave treatment at 500-700W for 10-15 minutes; the calcination process conditions are as follows: calcining at 500-600 ℃ for 2-3 hours.
5. The preparation method of claim 1, wherein the modified nanoparticles are prepared by the following steps in parts by weight: firstly, 1 part of N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane is dispersed in 5-7 parts of toluene by ultrasonic waves, then 0.4-0.6 part of aluminum silicate-calcium phosphate nanoparticles are added, the mixture is stirred and reacted for 6-8 hours at the temperature of 80-90 ℃, and the modified nanoparticles are obtained after centrifugation and drying.
6. An anchor rod grouting material for deep foundation pit construction, which is obtained by the preparation method of any one of claims 1-5.
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