CN116535132A - Retardation-promoting modified phosphate and preparation method and application thereof - Google Patents

Retardation-promoting modified phosphate and preparation method and application thereof Download PDF

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CN116535132A
CN116535132A CN202310813661.5A CN202310813661A CN116535132A CN 116535132 A CN116535132 A CN 116535132A CN 202310813661 A CN202310813661 A CN 202310813661A CN 116535132 A CN116535132 A CN 116535132A
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phosphate
parts
modified
cellulose ether
magnesium
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严煌
罗慧
洪量
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Guangdong Longhu Sci & Tech Co ltd
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Guangdong Longhu Sci & Tech Co ltd
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B40/00Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/0028Aspects relating to the mixing step of the mortar preparation
    • C04B40/0039Premixtures of ingredients
    • C04B40/0046Premixtures of ingredients characterised by their processing, e.g. sequence of mixing the ingredients when preparing the premixtures
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/34Compositions 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 cold phosphate binders
    • C04B28/344Compositions 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 cold phosphate binders the phosphate binder being present in the starting composition solely as one or more phosphates
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/20Retarders
    • C04B2103/22Set retarders
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/50Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/91Use of waste materials as fillers for mortars or concrete

Abstract

The invention provides a retarding modified phosphate and a preparation method and application thereof, wherein the preparation method of the modified phosphate is as follows: (1) mixing aluminum-silicon series admixture and phosphate according to the weight part of 1: (8-10) stirring and uniformly mixing to form mixed powder; (2) Will ρ -Al 2 O 3 The fine powder, the VAE emulsion and the water are mixed according to the weight parts of (10-20): (8-15): (4-8) mixing into a fluid mixture; (3) Pouring the fluid mixture prepared in the step (2) into the mixed powder prepared in the step (1) while stirring, wherein the weight ratio of the fluid mixture is (70-80): (20-30); (4) placing for 20-40 min at room temperature; (5) putting the mixture into a baking oven at 30-50 ℃ for drying; the retarding modified phosphate can be used for preparing phosphate cement repair mortar, and solves the problem of too fast setting time.

Description

Retardation-promoting modified phosphate and preparation method and application thereof
Technical Field
The invention belongs to the technical field of building materials, and particularly relates to a retarding-promoting modified phosphate, a preparation method and application thereof, which are mainly applied to pavement and bridge repair.
Background
The magnesium phosphate cement is usually prepared by taking magnesium oxide and phosphate as main components and compounding retarded components such as borax and the like according to a certain proportion, has the advantages of quick setting time, high early strength, good adhesive property, good volume stability, strong wear resistance and the like, is very suitable for being used as a cementing material of a quick repairing material in the field of building material markets, and is particularly suitable for small repairing of concrete pavement. The hardening mechanism is acid-base reaction, and a large amount of heat is released in the reaction process, so that the material is also very suitable for being used as a low-temperature repair material. However, the acid-base reaction is too rapid, the reaction speed is not well controlled, the setting time is very short, the operational time of the magnesium phosphate cement repair mortar which is mainstream in the market at present is less than 30min, some products are less than 10min, the magnesium phosphate cement repair mortar is suitable for structural rush repair of airport runways, highways, municipal main roads and the like, and along with the occurrence of carbonization and spalling problems and the like of concrete protection layers at special positions such as the elevation of structures in the service period, higher requirements are put on the fluidity, the setting time, the sagging resistance and the like of the magnesium phosphate mortar. The mixed use of both acidic and basic materials is also a significant challenge to the performance of conventional building material additives.
At present, most of researches on prolonging the setting time are to compound a plurality of retarders to retard the magnesium phosphate cement repair mortar. However, the compounding of the retarder has a certain influence on the working performance and the mechanical strength, the addition amount of the retarder which is not well controlled in the production process can greatly influence the construction performance and the mechanical property, the retarder effect cannot be achieved by adding a small amount of retarder, and the mechanical strength can be greatly reduced by adding excessive retarder.
The repair mortar is generally classified into two types of ground repair and elevation repair according to different construction sites. The fluidity, sagging resistance and other properties of the two repair mortars are respectively considered. The floor repair mortar needs to have better self-fluidity, and the facade repair mortar needs to have better sagging resistance. Conventional portland cement repair mortars generally employ the addition of building additives such as water reducers, cellulose ethers and starch ethers to achieve the desired workability. And the common building additives such as water reducing agent, cellulose ether and starch ether which can be practically applied to the magnesium phosphate cement repair mortar at the present stage are very few. The common water reducing agent, cellulose ether, starch ether and other building additives independently act on magnesium oxide to have the effects of dispersing, reducing water, preserving water and thickening respectively, but the building additives lose efficacy once phosphate is added, and the working performance of the building additives does not act any more.
The research shows that the polymer prolongs the setting time of the magnesium phosphate cement repair mortar through adsorption, relieves the occurrence rate of internal hydration reaction, and can improve the toughness of the magnesium phosphate cement repair mortar. As shown in the Studies of toughness mechanism of the polymer modified magnesium potassium phosphate cement, haiying, university of Fuzhou, 2017, the incorporation of VAE emulsion increases setting time of the magnesium potassium phosphate cement. However, if the system is used for the repairing mortar for the vertical face, a plurality of problems still exist, such as the magnesium phosphate cement repairing mortar added with the VAE emulsion still has larger fluidity, and the thickening and viscosity increasing effects of the additive cannot be exerted by adding the building additives such as starch ether, cellulose ether and the like into the system, so that the construction requirements of the repairing for the vertical face cannot be met. And the VAE emulsion is directly added, so that the influence on the setting time is limited, the VAE emulsion cannot be used as a retarder, or a large amount of retarders such as borax must be added to ensure that the magnesium phosphate cement repair mortar has reasonable setting time.
If the surface of the phosphate can be coated with a coating layer, the coating layer has a certain water-proof function, the dissolution speed of the phosphate in water is slowed down, the problem that the setting time is too fast can be solved, the problem that the phosphate causes the building additives such as a common water reducing agent, cellulose ether, starch ether and the like to fail can be solved, the prepared magnesium phosphate cement repair mortar can be used for floor repair, the types and the addition amount of the building additives in the formula can be regulated, the construction performance of the magnesium phosphate cement repair mortar meets the construction requirements of the facade repair mortar, and the application range of the magnesium phosphate cement repair mortar is expanded. However, the surface of the phosphate particles is smooth, and is generally difficult to directly coat by a physical method, and the coating layer is very easy to fall off. The method for modifying the phosphate particles is feasible, and great convenience can be provided for the phosphate cement repair mortar in the future.
Disclosure of Invention
Aiming at the problems of the technology, one of the purposes of the invention is to provide a modified phosphate for promoting the setting of retarder, which can be used for producing magnesium phosphate cement repair mortar, and plays a role of promoting the setting of retarder, so that the method for effectively prolonging the setting time of the magnesium phosphate cement repair mortar is provided on the premise of not adding excessive types of retarder, and the influence on the working performance and mechanical property of the magnesium phosphate cement repair mortar is reduced under the condition of meeting the construction operability. Meanwhile, the influence of phosphate on the building additive, especially on the common polycarboxylate water reducer, cellulose ether, starch ether and the like, is weakened, so that the building additive can restore the original working performance.
The second purpose of the invention is to provide the magnesium phosphate cement repair mortar for repairing the ground, and the modified phosphate is adopted, so that the cement repair mortar is short in setting time, good in fluidity and easy to construct.
The invention further aims to provide magnesium phosphate cement repair mortar for repairing the vertical surfaces, and the modified phosphate is short in setting time, good in sagging resistance and easy to construct.
In order to achieve the above purpose, the preparation method of the retarding modified phosphate comprises the following steps:
(1) Mixing aluminum-silicon series admixture and phosphate in parts by weight of 1: (8-10) mixing and stirring to ensure that the surfaces of the particles are fully wrapped by the superfine aluminum-silicon series admixture to form granular mixed powder;
(2) Will ρ -Al 2 O 3 The fine powder, the VAE emulsion and the water are mixed according to the weight parts of (10-20): (8-15): (4-8) uniformly mixing and stirring to form a fluid mixture;
(3) Pouring the fluid mixture prepared in the step (2) into the mixed powder prepared in the step (1) while stirring, wherein the mixed powder and the fluid mixture are mixed according to the weight ratio of (70-80): (20-30). Under the proportion, the superfine aluminum-silicon series admixture on the surface of the particles prepared in the step (1) can be quickly combined and adsorbed with the mixture in the step (2) to form a mixture taking phosphate as a core, and the surface of the mixture is coated with the aluminum-silicon series admixture and rho-Al 2 O 3 The fines and VAE are packed into a loose mixture of shells; if the dosage of the fluid mixture is too high, the formed shell is too thick, water needs to permeate into the shell for a longer time to dissolve phosphate, the coagulation time is too long, if the dosage of the fluid mixture is too low, a continuous shell cannot be formed, the phosphate is dissolved when the water contacts with the phosphate, and the water-proof effect cannot be achieved;
(4) Placing the phosphate particles forming the uniform coating layer at room temperature for 20-40 min to enable rho-Al on the surfaces of the phosphate particles to be 2 O 3 Hydration to form Al (OH) 3 ;Al(OH) 3 React with phosphate to form AlPO 4 The precipitation coats the surface of the phosphate particles, and this reaction promotes ρ -Al on the surface of the phosphate particles 2 O 3 Further hydration, to form more gelatinous diaspore and boehmite gels, which form a rough and hard coating that reacts in situ. Simultaneous ρ -Al 2 O 3 Hydration and water absorption enable a part of VAE emulsion to form a film in the rough coating layer, improve the interface effect and enable the coating layer to be firmly adhered on the surface of the phosphate particles;
(5) Drying in a 30-50deg.C oven to obtain a film with the VAE emulsion which is not dried on the surface of the granule, and has reduced water content, and is suitable for storage and use. Completely drying to obtain phosphate particles as core, mixing with Al-Si system, and ρ -Al 2 O 3 The mixture of the product of hydration reaction of the fine powder and the VAE emulsion is the modified phosphate particles of the shell. The modified phosphate particles have the characteristics of easy storage, controllable reaction speed, simple preparation process, economy and practicability.
Preferably, the phosphate in the step (1) is one or two selected from monoammonium phosphate and monopotassium phosphate.
Preferably, the mesh number of the phosphate in the step (1) is 40-100 meshes, the phosphate content is more than or equal to 99.0%, and the pH value of a phosphate solution with the mass concentration of 1% is less than 5.
Preferably, step (2) the ρ -Al 2 O 3 The granularity of the fine powder is 50-100 mu m, al 2 O 3 The content is more than 90 percent.
Preferably, the VAE emulsion in the step (2) is a VAE emulsion with a glass transition temperature of-5-20 ℃, a solid content of 50-57%, an ethylene content of 25-30% and no free formaldehyde.
Preferably, the aluminum-silicon series admixture is one of superfine fly ash, slag or silica fume with fine powder granularity smaller than 10 mu m; the aluminum-silicon series admixture plays a role in the step (1) of adsorbing the VAE emulsion and furtherEasy to be matched with rho-Al 2 O 3 The fine powder jointly acts to coat the surface of the phosphate particles.
The delayed coagulation promoting modified phosphate can be used for producing magnesium phosphate cement repair mortar for the ground, and is prepared from the following components in parts by weight:
25-35 parts of magnesium oxide, 15-25 parts of modified phosphate, 10-15 parts of fly ash microbeads, 3-8 parts of aluminum-silicon series admixture, 30-40 parts of quartz sand, 1-3 parts of borax and 0.13-0.28 part of additive A.
The retarding modified phosphate can also be used for producing magnesium phosphate cement repair mortar for facades, and is prepared from the following components in parts by weight:
25-35 parts of magnesium oxide, 15-25 parts of modified phosphate, 10-15 parts of fly ash microbeads, 35-45 parts of quartz sand, 1-5 parts of borax and 0.05-0.10 part of additive B.
The components in the repair mortar are uniformly mixed for use.
Preferably, the magnesia is formed by crushing burned magnesia, and the specific surface area is 240-300 m 2 /kg。
Preferably, the fly ash microbeads d 50 The shape of the mortar is less than or equal to 3 mu m, and the mortar is in a standard sphere shape, so that the mortar has the effects of providing microbead effect for the magnesium phosphate cement repair mortar, reducing water addition, improving construction performance and increasing strength.
Preferably, the aluminum-silicon series admixture is one of superfine fly ash, slag or silica fume with fine powder granularity smaller than 10 mu m; the aluminum-silicon series admixture plays a role in magnesium phosphate cement repair mortar finished product mixture, and is used as an ultrafine active filler to improve the mechanical strength of the repair mortar.
Preferably, the quartz sand is 10-150 mesh.
Preferably, the borax is borax decahydrate, wherein Na 2 B 4 O 7 •10H 2 The O content is more than or equal to 99.0 percent.
Preferably, the additive A is a polycarboxylic acid type water reducer and cellulose ether compound. Wherein the water reducing rate of the polycarboxylic acid type water reducer is more than or equal to 20 percent, and the addition amount is 0.05 to 0.13 part; the cellulose ether is one of hydroxyethyl methyl and hydroxypropyl methyl cellulose ether, the NDJ viscosity is 300-600 mPa.s, and the addition amount is 0.08-0.15 part.
Preferably, the additive B is a cellulose ether and thickener compound. Wherein the cellulose ether is hydroxyethyl methyl or hydroxypropyl methyl cellulose ether, the NDJ viscosity range is 40000-70000 mPa.s, and the addition amount is 0.04-0.10 parts; the thickener is one of starch ether, guar gum or xanthan gum. Preferably, the starch ether is potato starch ether, and the fineness is less than or equal to 0.5mm; the NDJ viscosity of the guar gum 1% aqueous solution is more than or equal to 5000 mPa.s; the viscosity of the 1% aqueous solution of the xanthan gum Brook field is more than or equal to 600cP.
Preferably, the additive B is cellulose ether 0.02-0.05 part and potato starch ether 0.03-0.05 part; the cellulose ether is one of hydroxyethyl methyl cellulose ether or hydroxypropyl methyl cellulose ether, and the NDJ viscosity is 40000-70000 mPa.s.
After the modified phosphate particles are mixed with water, the shell on the surface of the phosphate particles is gradually destroyed in the mechanical stirring process, so that the phosphate is gradually dissolved out. In the process, due to the barrier property of the shell, the phosphate particles are not immediately dissolved and dispersed, but are slowly decomposed under the action of water penetration, so that the construction time of the phosphate repair mortar can be prolonged, and the construction additives in the phosphate repair mortar, especially the common polycarboxylate water reducer, cellulose ether, starch ether and the like, can maintain the original working performance within the construction time of the phosphate repair mortar.
Compared with the prior art, the invention has the following beneficial effects:
adopts the physical and chemical method to adsorb the VAE emulsion by the ultrafine powder particles, and then the VAE emulsion is processed by rho-Al 2 O 3 The surface of the phosphate particles is modified by the hydration reaction of the fine powder, and the surface of the phosphate particles is coated into a shell under the combined action, so that the dissolution rate of the phosphate is greatly reduced, and the problem of too fast setting time of the magnesium phosphate cement repair mortar is solved. Meanwhile, the slowly dissolved phosphate also prolongs the dispersing, water reducing, water retaining and thickening effects of building additives such as common polycarboxylate water reducer, cellulose ether, starch ether and the like on the magnesium phosphate cement repair mortar, and improves the magnesium phosphate cement repair effectAnd (5) the construction property of the mortar. The method is easy to store, has controllable reaction speed, simple preparation process, economy and practicability and is convenient for large-scale industrial application. In addition, spherical fly ash particles with smaller average particle size are used as micro aggregates to be filled among other powder particles with larger particle size, so that better grading collocation is formed, the physical water reducing effect is achieved, the pore structure of the repair mortar is improved, and the strength is increased.
Detailed Description
The present invention will be described in further detail with reference to the following embodiments. The following examples will assist those skilled in the art in further understanding the present invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications could be made by those skilled in the art without departing from the inventive concept. These are all within the scope of the present invention.
The raw materials used in the examples are described below:
the magnesia is formed by crushing burned magnesia, and the specific surface area is 240-300 m 2 /kg; the mesh number of the ammonium dihydrogen phosphate is 40-100 meshes, and NH 4 H 2 PO 4 The content is more than or equal to 99.0 percent, and the pH value of the ammonium dihydrogen phosphate aqueous solution with the mass concentration of 1 percent is less than 5; the mesh number of the monopotassium phosphate is 40-100 meshes, KH 2 PO 4 The content is more than or equal to 99.0 percent, and the pH value of a1 percent potassium dihydrogen phosphate aqueous solution with the mass concentration is less than 5; said ρ -Al 2 O 3 The granularity of the fine powder is 50-100 mu m, al 2 O 3 The content is more than 90 percent; the solid content of the VAE emulsion is 54.5-56.5%, and the brand is VINNAPAS 547 ED; the fly ash microbead d 50 The size is less than or equal to 3 mu m, and the shape is standard sphere; the aluminum-silicon series admixture is superfine fly ash with fineness less than 10 mu m; the quartz sand is 10-150 meshes; borax is borax decahydrate, wherein Na 2 B 4 O 7 •10H 2 The O content is more than or equal to 99.0 percent; the water reducing rate of the polycarboxylic acid type water reducing agent is more than or equal to 20%, and the polycarboxylic acid type water reducing agent Hanrius P29 is provided by Guangdong lake technology Co., ltd; the hydroxypropyl methyl cellulose ether is hydroxypropyl methyl cellulose ether marcchem HPMC500 provided by Guangdong lake science and technology Co., ltd, and the NDJ viscosity range is 300-600 mPa.s; hydroxyethyl groupThe methyl cellulose ether is hydroxyethyl methyl cellulose ether Tylose MH60001P6 provided by Guangdong lake science and technology Co., ltd, and the NDJ viscosity range is 40000-70000 mPa.s; the potato starch ether is potato starch ether Opagel CMT provided by Guangdong lake technology Co.
Examples of modified monoammonium phosphate are as follows.
Example 1
The retarding modified monoammonium phosphate A is prepared according to the following steps:
(1) Mixing aluminum-silicon series admixture and monoammonium phosphate according to the weight part of 1:8, adding the mixture into stirring equipment and stirring the mixture into uniform mixed powder;
(2) Will ρ -Al 2 O 3 The fine powder, the VAE emulsion and the water are prepared according to the weight parts of 12:8:5, mixing and stirring uniformly to form a fluid mixture;
(3) Pouring all the uniform mixed powder prepared in the step (1) into a stirrer, and pouring the fluidized mixture prepared in the step (2) while stirring, wherein the weight ratio of the uniform mixed powder to the fluidized mixture is 75:25, stirring to form a mixture with ammonium dihydrogen phosphate as a core and aluminum-silicon series admixture and rho-Al on the surface 2 O 3 The fines and VAE are packed into a loose mixture of shells;
(4) Standing at room temperature for 30min to obtain ρ -Al 2 O 3 Hydrated with NH on the surface of monoammonium phosphate particles 4 H 2 PO 4 A chemical reaction occurs;
(5) And (5) putting the mixture into a baking oven at 40 ℃ for baking to obtain modified monoammonium phosphate A particles.
Example 2
The retarding modified monoammonium phosphate B is prepared according to the following steps:
(1) Mixing aluminum-silicon series admixture and monoammonium phosphate according to the weight part of 1:9, adding the mixture into stirring equipment and stirring the mixture into uniform mixed powder;
(2) Will ρ -Al 2 O 3 The fine powder, the VAE emulsion and the water are prepared according to the weight parts of 12:7:6, mixing and stirring uniformly to form a fluid mixture;
(3) Pouring all the uniform mixed powder prepared in the step (1) into a stirrer while stirringPouring the fluidized mixture prepared in the step (2) while stirring, wherein the weight ratio of the uniform mixed powder to the fluidized mixture is 75:25. stirring to form a mixture with ammonium dihydrogen phosphate as core and aluminum-silicon series doped material and rho-Al on the surface 2 O 3 The fines and VAE are packed into a loose mixture of shells;
(4) Standing at room temperature for 30min to obtain ρ -Al 2 O 3 Hydrated with NH on the surface of monoammonium phosphate particles 4 H 2 PO 4 A chemical reaction occurs;
(5) And (5) putting the mixture into a baking oven at 40 ℃ for baking to obtain modified monoammonium phosphate B particles.
Example 3
The retarding modified monoammonium phosphate C is prepared according to the following steps:
(1) Mixing aluminum-silicon series admixture and monoammonium phosphate according to the weight part of 1:10, adding the mixture into stirring equipment and stirring the mixture into uniform mixed powder;
(2) Will ρ -Al 2 O 3 The fine powder, the VAE emulsion and the water are prepared according to the weight parts of 12:6:7, mixing and stirring uniformly to form a fluid mixture;
(3) Pouring all the uniform mixed powder prepared in the step (1) into a stirrer, and pouring the fluidized mixture prepared in the step (2) while stirring, wherein the weight ratio of the uniform mixed powder to the fluidized mixture is 75:25. stirring to form a mixture with ammonium dihydrogen phosphate as core and aluminum-silicon series doped material and rho-Al on the surface 2 O 3 The fines and VAE are packed into a loose mixture of shells;
(4) Standing at room temperature for 30min to obtain ρ -Al 2 O 3 Hydrated with NH on the surface of monoammonium phosphate particles 4 H 2 PO 4 A chemical reaction occurs;
(5) And (5) putting the mixture into a baking oven at 40 ℃ for baking to obtain modified monoammonium phosphate C particles.
Example 4
The retarding modified potassium dihydrogen phosphate is prepared according to the following steps:
(1) Mixing aluminum-silicon series admixture and monopotassium phosphate according to the weight part of 1:9, adding the mixture into stirring equipment and stirring the mixture into uniform mixed powder;
(2) Will ρ -Al 2 O 3 The fine powder, the VAE emulsion and the water are prepared according to the weight parts of 12:7:6, mixing and stirring uniformly to form a fluid mixture;
(3) Pouring all the uniform mixed powder prepared in the step (1) into a stirrer, and pouring the fluidized mixture prepared in the step (2) while stirring, wherein the weight ratio of the uniform mixed powder to the fluidized mixture is 75:25. stirring to form a mixture with potassium dihydrogen phosphate as core and aluminum-silicon series doped material and rho-Al on the surface 2 O 3 The fines and VAE are packed into a loose mixture of shells;
(4) Standing at room temperature for 30min to obtain ρ -Al 2 O 3 Hydrating the surface of the potassium dihydrogen phosphate particles and carrying out chemical reaction with the potassium dihydrogen phosphate;
(5) And (5) putting the mixture into a baking oven at 40 ℃ for baking to obtain modified potassium dihydrogen phosphate particles.
Examples 5 to 7 below are application examples of modified phosphate to magnesium phosphate cement repair mortar for floor repair (parts thereof are Kg).
Example 5
The magnesium phosphate cement repair mortar for repairing the ground is mainly prepared from the following raw materials in parts by weight:
33 parts of magnesium oxide, 17 parts of modified monoammonium phosphate A, 10 parts of fly ash microbeads, 5 parts of aluminum-silicon series admixture, 35 parts of quartz sand, 2 parts of borax, 0.05 part of polycarboxylate water reducer (P29) and 0.03 part of hydroxypropyl methyl cellulose ether (HPMC 500).
Example 6
The magnesium phosphate cement repair mortar for repairing the ground is mainly prepared from the following raw materials in parts by weight:
30 parts of magnesium oxide, 19 parts of modified monoammonium phosphate B, 10 parts of fly ash microbeads, 5 parts of aluminum-silicon series admixture, 36 parts of quartz sand, 2 parts of borax, 0.04 part of polycarboxylate water reducer (P29) and 0.03 part of hydroxypropyl methyl cellulose ether (HPMC 500).
Example 7
The magnesium phosphate cement repair mortar for repairing the ground is mainly prepared from the following raw materials in parts by weight:
26 parts of magnesium oxide, 21 parts of modified monoammonium phosphate, 10 parts of fly ash microbeads, 5 parts of aluminum-silicon series admixture, 38 parts of quartz sand, 2 parts of borax, 0.04 part of polycarboxylate water reducer (P29) and 0.03 part of hydroxypropyl methyl cellulose ether (HPMC 500).
Comparative example 1
Except that ammonium dihydrogen phosphate is not modified, the specific formulation is as follows, except that the method is as follows:
30 parts of magnesium oxide, 19 parts of ammonium dihydrogen phosphate, 10 parts of fly ash microbeads, 5 parts of aluminum-silicon series admixture, 36 parts of quartz sand, 2 parts of borax, 0.04 part of polycarboxylate water reducer (P29) and 0.03 part of hydroxypropyl methyl cellulose ether (HPMC 500).
Comparative example 2
Except that ammonium dihydrogen phosphate is not modified, the addition amount of borax is changed to 6 parts, and the specific formula is as follows in the example 6:
30 parts of magnesium oxide, 19 parts of ammonium dihydrogen phosphate, 10 parts of fly ash microbeads, 5 parts of aluminum-silicon series admixture, 36 parts of quartz sand, 6 parts of borax, 0.04 part of polycarboxylate water reducer (P29) and 0.03 part of hydroxypropyl methyl cellulose ether (HPMC 500).
Performance detection
Examples 5 to 7 and comparative examples 1 to 2 were subjected to performance test according to JC/T2537-2019 magnesium phosphate repair mortar. The test performance results are shown in Table 1.
As can be seen from comparative example 6, comparative example 1 and comparative example 2, the modified monoammonium phosphate particles of the invention can bring the original working performance of the ordinary polycarboxylate superplasticizer into play, effectively improve the fluidity of the magnesium phosphate cement repair mortar, prolong the setting time and have little influence on the mechanical properties. The fluidity of the magnesium phosphate cement repair mortar can be effectively increased by increasing the addition amount of borax, and the setting time is prolonged, but the mechanical property of the magnesium phosphate cement repair mortar test block in the later stage is obviously adversely affected.
Examples 8 to 11 below are application examples of modified phosphate for magnesium phosphate cement repair mortar for facades (wherein the parts are Kg).
Example 8
28 parts of magnesium oxide, 18 parts of modified monoammonium phosphate B, 14 parts of fly ash microbeads, 40 parts of quartz sand, 2 parts of borax, 0.05 part of hydroxyethyl methyl cellulose ether (MH 60001P 6) and 0.03 part of potato starch ether (Opgel CMT).
Example 9
28 parts of magnesium oxide, 18 parts of modified potassium dihydrogen phosphate, 14 parts of fly ash microbeads, 40 parts of quartz sand, 2 parts of borax, 0.05 part of hydroxyethyl methyl cellulose ether (MH 60001P 6) and 0.03 part of potato starch ether (Opgel CMT).
Example 10
28 parts of magnesium oxide, 18 parts of modified monoammonium phosphate A, 14 parts of fly ash microbeads, 40 parts of quartz sand, 2 parts of borax, 0.05 part of hydroxyethyl methyl cellulose ether (MH 60001P 6) and 0.03 part of potato starch ether (Opgel CMT).
Example 11
30 parts of magnesium oxide, 19 parts of modified monoammonium phosphate B, 12 parts of fly ash microbeads, 45 parts of quartz sand, 1 part of borax, 0.04 part of hydroxyethyl methyl cellulose ether (MH 60001P 6) and 0.04 part of potato starch ether (Opgel CMT).
Comparative example 3
Except that ammonium dihydrogen phosphate is not modified, the specific formulation is as follows, except that the method is as follows in example 8:
28 parts of magnesium oxide, 18 parts of monoammonium phosphate, 14 parts of fly ash microbeads, 40 parts of quartz sand, 2 parts of borax, 0.05 part of hydroxyethyl methyl cellulose ether (MH 60001P 6) and 0.03 part of potato starch ether (Opgel CMT).
Comparative example 4
Except that ammonium dihydrogen phosphate is not modified, the addition amount of borax is changed to 6 parts, and the rest is the same as in example 8, and the specific formula is as follows:
28 parts of magnesium oxide, 18 parts of monoammonium phosphate, 14 parts of fly ash microbeads, 40 parts of quartz sand, 6 parts of borax, 0.05 part of hydroxyethyl methyl cellulose ether (MH 60001P 6) and 0.03 part of potato starch ether (Opgel CMT).
Examples 8-11 and comparative examples 3-4 were tested for performance according to JC/T2537-2019 magnesium phosphate repair mortar and tested for sagging. The test performance results are shown in Table 2.
As can be seen from comparative examples 8 and 3-4, the modified phosphate of the invention can bring the original working performance into play after the cellulose ether and the starch ether are compounded, and obviously improves the viscosity of the magnesium phosphate cement repair mortar, thereby improving the sagging resistance, prolonging the setting time, having little influence on the mechanical properties and ensuring that the magnesium phosphate cement repair mortar can perform normal elevation construction. The setting time can be effectively prolonged by increasing the addition amount of the borax, but as the fluidity of the magnesium phosphate cement repair mortar can be increased by the borax, and meanwhile, the thickening and viscosity increasing performances of the magnesium phosphate cement repair mortar are weakened under the action of unmodified phosphate after the cellulose ether and the starch ether are compounded, so that the magnesium phosphate cement repair mortar has excellent self-fluidity and cannot be subjected to elevation construction.
In the present invention, the percentage content is not specifically described as the weight percentage content.
The protective scope of the invention is not limited to the embodiments described above, but it will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the scope and spirit of the invention. It is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.

Claims (10)

1. The preparation method of the retarding-promoting modified phosphate is characterized by comprising the following steps of:
(1) Mixing aluminum-silicon series admixture and phosphate in parts by weight of 1: (8-10) mixing and stirring to form granular mixed powder;
(2) Will ρ -Al 2 O 3 The fine powder, the VAE emulsion and the water are mixed according to the weight parts of (10-20): (8-15): (4-8) uniformly mixing and stirring to form a fluid mixture;
(3) Pouring the fluid mixture prepared in the step (2) into the mixed powder prepared in the step (1) while stirring, wherein the mixed powder and the fluid mixture are mixed according to the weight ratio of (70-80): (20-30); forming phosphate particles having a coating layer;
(4) Placing the phosphate particles with the coating layer at room temperature for 20-40 min;
(5) And then drying at 30-50 ℃ to obtain the retarding modified phosphate.
2. The method for preparing a modified delayed coagulation promoting phosphate according to claim 1, wherein the phosphate in the step (1) is one or two selected from monoammonium phosphate and monopotassium phosphate.
3. The method for preparing a modified delayed coagulation promoting phosphate according to claim 1 or 2, wherein the mesh number of the phosphate in the step (1) is 40-100 mesh, and the phosphate content is more than or equal to 99.0%.
4. The method for producing a retarder-promoting modified phosphate according to claim 1, wherein the ρ -Al is as defined in step (2) 2 O 3 The granularity of the fine powder is 50-100 mu m, al 2 O 3 The content is more than 90 percent; the VAE emulsion is a VAE emulsion with a glass transition temperature of-5-20 ℃, a solid content of 50-57% and an ethylene content of 25-30%.
5. The method for preparing the retarding modified phosphate according to claim 1, wherein the aluminum-silicon series admixture is one of superfine fly ash, slag or silica fume with fine powder granularity less than 10 mu m.
6. Retarder-promoting modified phosphate prepared by the preparation method according to any one of claims 1 to 5.
7. The magnesium phosphate cement repair mortar for the ground prepared by adopting the retarding modified phosphate as defined in claim 6 is characterized by comprising the following components in parts by weight: 25-35 parts of magnesium oxide, 15-25 parts of modified phosphate, 10-15 parts of fly ash microbeads, 3-8 parts of aluminum-silicon series admixture, 30-40 parts of quartz sand, 1-3 parts of borax and 0.13-0.28 part of additive A.
8. The magnesium phosphate cement repair mortar for the ground according to claim 7, wherein the additive A is a polycarboxylic acid type water reducing agent and cellulose ether, wherein the water reducing rate of the polycarboxylic acid type water reducing agent is more than or equal to 20%, and the addition amount is 0.05-0.13 part; the cellulose ether is one of hydroxyethyl methyl cellulose ether and hydroxypropyl methyl cellulose ether, the NDJ viscosity range is 300-600 mPa.s, and the addition amount is 0.08-0.15 part.
9. The magnesium phosphate cement repair mortar for facades prepared by adopting the retarding modified phosphate as defined in claim 6 is characterized by comprising the following components in parts by weight: 25-35 parts of magnesium oxide, 15-25 parts of modified phosphate, 10-15 parts of fly ash microbeads, 35-45 parts of quartz sand, 1-3 parts of borax and 0.05-0.10 part of additive B.
10. The magnesium phosphate cement repair mortar for facades according to claim 9, characterized in that the additive B is cellulose ether 0.02-0.05 parts, potato starch ether 0.03-0.05 parts; the cellulose ether is one of hydroxyethyl methyl cellulose ether or hydroxypropyl methyl cellulose ether, and the NDJ viscosity is 40000-70000 mPa.s.
CN202310813661.5A 2023-07-05 2023-07-05 Retardation-promoting modified phosphate and preparation method and application thereof Pending CN116535132A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2126521A1 (en) * 1970-06-02 1971-12-16 Chvatal T Phosphate -base binder - with siliceous absorber for refractory mater
KR20040016049A (en) * 2002-08-14 2004-02-21 주식회사 지구와사람 Flame retardantion polyethylen terephalate use of phoshorus flame retardants and a manufacturing proecess
CN106186976A (en) * 2016-07-14 2016-12-07 济南大学 A kind of condensation controllable type complex cement base sealing material and application process thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2126521A1 (en) * 1970-06-02 1971-12-16 Chvatal T Phosphate -base binder - with siliceous absorber for refractory mater
KR20040016049A (en) * 2002-08-14 2004-02-21 주식회사 지구와사람 Flame retardantion polyethylen terephalate use of phoshorus flame retardants and a manufacturing proecess
CN106186976A (en) * 2016-07-14 2016-12-07 济南大学 A kind of condensation controllable type complex cement base sealing material and application process thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
契尔金斯基等: "《聚合物水泥混凝土 增订第2版》", vol. 1, 中国建筑工业出版社, pages: 165 - 160 *

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