CN118993662B - A high-strength fireproof mortar and its preparation process - Google Patents

A high-strength fireproof mortar and its preparation process Download PDF

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CN118993662B
CN118993662B CN202411081499.3A CN202411081499A CN118993662B CN 118993662 B CN118993662 B CN 118993662B CN 202411081499 A CN202411081499 A CN 202411081499A CN 118993662 B CN118993662 B CN 118993662B
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aluminum hydroxide
mixing
flame retardant
vinyl
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CN118993662A (en
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龙专
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Hainan Ruichen New Building Materials Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/06Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
    • C08F283/065Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
    • 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
    • C04B28/02Compositions 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
    • C04B28/06Aluminous cements
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/12Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes
    • C08F283/124Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes on to polysiloxanes having carbon-to-carbon double bonds
    • 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
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00482Coating or impregnation materials
    • C04B2111/00525Coating or impregnation materials for metallic surfaces
    • 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
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20Resistance against chemical, physical or biological attack
    • C04B2111/28Fire resistance, i.e. materials resistant to accidental fires or high temperatures
    • 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
    • C04B2201/10Mortars, concrete or artificial stone characterised by specific physical values for the viscosity
    • 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
    • C04B2201/30Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
    • C04B2201/32Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
    • 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

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Fireproofing Substances (AREA)

Abstract

本发明涉及砂浆领域,具体是一种高强防火砂浆及其制备工艺,以氢氧化铝作为阻燃剂,对氢氧化铝进行改性处理,先用(3‑巯基丙基)三甲氧基硅烷使其表面巯基化,然后利用巯基‑双键的光点击,在其表面引入含有双键的阻燃单体、乙烯基支化聚硅氧烷;含有双键的阻燃单体为采用甲基丙烯酸缩水甘油酯对小分子阻燃剂一磷酸腺苷进行改性制备的阻燃单体;而乙烯基支化聚硅氧烷为一缩二丙二醇、乙烯基三乙氧基硅烷合成含有大量Si‑O键、双键的超支化聚硅氧烷;以高效聚羧酸减水剂原料烯丙基聚氧乙烯醚为主链,接枝反应活性强的乙烯基支化聚硅氧烷和亲水性强的丙烯酸,制备强亲水性、高反应活性和高减水效果的有机硅改性聚羧酸减水剂。The invention relates to the field of mortar, in particular to a high-strength fireproof mortar and a preparation process thereof. Aluminum hydroxide is used as a flame retardant, and the aluminum hydroxide is modified. First, (3-mercaptopropyl) trimethoxysilane is used to thiolize the surface of the aluminum hydroxide, and then a flame retardant monomer containing double bonds and a vinyl branched polysiloxane are introduced on the surface of the aluminum hydroxide by photo-clicking of the mercapto-double bonds. The flame retardant monomer containing double bonds is a flame retardant monomer prepared by modifying a small molecule flame retardant adenosine monophosphate with glycidyl methacrylate. The vinyl branched polysiloxane is a hyperbranched polysiloxane containing a large number of Si-O bonds and double bonds synthesized from dipropylene glycol and vinyl triethoxysilane. Allyl polyoxyethylene ether, a raw material of a high-efficiency polycarboxylic acid water reducer, is used as the main chain, and vinyl branched polysiloxane with strong grafting reaction activity and acrylic acid with strong hydrophilicity are used to prepare an organosilicon-modified polycarboxylic acid water reducer with strong hydrophilicity, high reaction activity and high water reduction effect.

Description

High-strength fireproof mortar and preparation process thereof
Technical Field
The invention relates to the field of mortar, in particular to high-strength fireproof mortar and a preparation process thereof.
Background
The diversity of building materials adds bricks and tiles to the social development, with the consequent safety problem, especially today in power society, fire is a major concern for safety problems.
The existing building mostly adopts a steel structure with quick heat conduction, and has the problems that the mechanical property, the bearing capacity and the like are rapidly reduced along with the temperature rise, and the like. Therefore, the fireproof protection measures are necessary means for the steel structure building, such as adopting a heat-insulating fireproof mortar material to improve the fireproof performance of the building, while the traditional cement mortar has the defects of higher self density, low strength, easy hollowing and falling off when meeting fire and the like, and cannot meet the requirements of special places such as oil stations, wharfs and the like on fireproof heat insulation.
Disclosure of Invention
The invention aims to provide high-strength fireproof mortar and a preparation process thereof, so as to solve the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
The high-strength fireproof mortar comprises, by mass, 100-150 parts of silicate cement, 115-150 parts of sulphoaluminate refractory cement, 15-30 parts of silica powder, 8-20 parts of redispersible latex powder, 2.5-4.8 parts of auxiliary agent, 100-150 parts of vermiculite sand, 460-580 parts of volcanic rock and 40-80 parts of flame retardant.
Further, the volcanic rock has a particle size of 30-100 meshes and a bulk density of 500-550kg/m 3.
Further, the flame retardant is aluminum hydroxide.
Further, the auxiliary agent is formed by compounding (1.8-3) thickener, air entraining agent, retarder and water reducer (0.1-0.4) and (0.1-0.4) in a mass ratio of (0.5-1).
Further, the thickener is hydroxypropyl cellulose ether, the air entraining agent is alpha-sodium alkenyl sulfonate, and the retarder is sodium gluconate.
Further, the water reducer is a polycarboxylate water reducer.
Further, the water reducer is an organosilicon modified polycarboxylate water reducer, and the preparation method comprises the following steps:
Mixing allyl polyoxyethylene ether and vinyl branched polysiloxane, adding a mixed solution of deionized water, acrylic acid and potassium persulfate, heating to 78-82 ℃, preserving heat for 4-5h, cooling, dialyzing with deionized water for 2d, and drying to obtain the organosilicon modified polycarboxylate water reducer.
Further, the flame retardant is composite aluminum hydroxide, and the preparation method comprises the following steps:
(1) Mixing aluminum hydroxide and ethanol, adding (3-mercaptopropyl) trimethoxy silane, preserving heat for 10-12h at 48-52 ℃, filtering, washing, drying and grinding to obtain mercaptoaluminum hydroxide;
(2) Mixing adenosine monophosphate and dimethyl sulfoxide, adding hydrochloric acid, adding glycidyl methacrylate, heating to 90-95 ℃ and preserving heat for 6-7h, adding ethyl acetate, filtering, washing and drying to obtain a flame-retardant monomer containing double bonds;
(3) Mixing vinyl branched polysiloxane, a double bond-containing flame-retardant monomer and sulfhydrylated aluminum hydroxide, adding a mixed solution of benzoin dimethyl ether and tetrahydrofuran, irradiating for 20-30min under an ultraviolet lamp with the wavelength of 325nm, performing rotary evaporation, adding petroleum ether, filtering, performing rotary evaporation, and drying to obtain the composite aluminum hydroxide.
Further, the preparation of the vinyl branched polysiloxane comprises the following steps of mixing dipropylene glycol and vinyl triethoxysilane under nitrogen atmosphere, adding barium hydroxide, heating to 78-82 ℃ until the system is clear, heating to 118-122 ℃ and preserving heat for 8-12min, continuing to preserve heat for 3-4h, cooling and filtering to obtain the vinyl branched polysiloxane.
Further, the preparation process of the high-strength fireproof mortar comprises the following steps of mixing silicate cement, sulphoaluminate refractory cement, silica powder and vermiculite sand, adding redispersible latex powder, an auxiliary agent and a flame retardant, mixing and stirring, adding volcanic rock, and continuing stirring to obtain the high-strength fireproof mortar.
The invention has the beneficial effects that:
The invention provides high-strength fireproof mortar and a preparation process thereof, and the high-strength fireproof mortar is high in strength and excellent in cohesiveness, fireproof heat insulation and corrosion resistance through component and proportion design.
The mortar has the advantages of high strength, low density, low heat conductivity and the like by adding the fire-proof material vermiculite sand into the mortar, the volcanic rock is used as a filler, gaps are generated in a porous system by controlling the particle size of the volcanic rock to play a role in heat insulation, silicon powder is added as an admixture to reduce the water-material ratio, so that the strength is enhanced, and the redispersible latex powder is selected as an adhesive material, so that the prepared mortar has the characteristics of flame resistance, low smoke, no toxicity, good elasticity, corrosion resistance and the like.
In order to improve the fireproof flame retardance of mortar, aluminum hydroxide is used as an environment-friendly flame retardant, and in order to solve the problems of high hydrophilicity and polarity contained on the surface of aluminum hydroxide, poor dispersity and compatibility in mortar, easy aggregation and the like, the invention carries out modification treatment on the aluminum hydroxide, firstly (3-mercaptopropyl) trimethoxysilane is used for carrying out surface sulfhydrylation on the aluminum hydroxide, then a flame-retardant monomer containing double bonds and vinyl branched polysiloxane are introduced on the surface of the aluminum hydroxide by utilizing light-spot of the mercapto-double bonds, so that the aluminum hydroxide plays a role of synergistic flame retardance and fire prevention under the action of the flame-retardant monomer containing double bonds and the vinyl branched polysiloxane, wherein the flame-retardant monomer containing double bonds is a flame-retardant monomer prepared by modifying micromolecular flame retardant adenosine monophosphate by adopting glycidyl methacrylate; the vinyl branched polysiloxane is hyperbranched polysiloxane which is synthesized by dipropylene glycol and vinyl triethoxysilane and contains a large amount of Si-O bonds and double bonds, and has the effects of flame retardance and fire prevention, and meanwhile, the anti-chloride ion permeability of the mortar is greatly improved, the drying shrinkage is reduced, and the flexural strength of the mortar is improved.
According to the invention, the high-efficiency polycarboxylate water reducer raw material allyl polyoxyethylene ether is taken as a main chain, vinyl branched polysiloxane with strong grafting reaction activity and acrylic acid with strong hydrophilicity are used for preparing the organosilicon modified polycarboxylate water reducer with strong hydrophilicity, high reaction activity and high water reducing effect, so that the bonding strength and corrosion resistance of mortar are improved, and the service life of the mortar is prolonged.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that, if directional indications such as up, down, left, right, front, and rear are involved in the embodiment of the present invention, the directional indication is merely used to explain a relative positional relationship between a specific posture such as each component, a movement condition, and the like, and if the specific posture is changed, the directional indication is changed accordingly. In addition, the technical solutions of the embodiments may be combined with each other, but it is necessary to base that the technical solutions can be realized by those skilled in the art, and when the technical solutions are contradictory or cannot be realized, the combination of the technical solutions should be considered to be absent and not within the scope of protection claimed in the present invention.
The following description of the embodiments of the present invention will be presented in further detail with reference to the examples, which should be understood as being merely illustrative of the present invention and not limiting.
The embodiment 1 is a preparation process of high-strength fireproof mortar, which comprises the following steps of mixing silicate cement, sulphoaluminate refractory cement, silica powder and vermiculite sand, adding redispersible latex powder, an auxiliary agent and a flame retardant, mixing and stirring, adding volcanic rock, and continuing stirring to obtain the high-strength fireproof mortar;
The mortar comprises 130 parts of silicate cement, 120 parts of sulphoaluminate refractory cement, 25 parts of silica powder, 15 parts of redispersible emulsion powder, 3.9 parts of auxiliary agent, 132 parts of vermiculite sand, 520 parts of volcanic rock and 62 parts of flame retardant;
The volcanic rock particle size is 80 meshes, the stacking density is 520kg/m 3, the flame retardant is aluminum hydroxide, the auxiliary agent is a thickening agent, an air entraining agent, a retarder and a water reducing agent, wherein the thickening agent is hydroxypropyl cellulose ether, the air entraining agent is alpha-sodium alkenyl sulfonate, the retarder is sodium gluconate, and the water reducing agent is a polycarboxylate water reducing agent.
The embodiment 2 is a preparation process of the high-strength fireproof mortar, which comprises the following steps of mixing silicate cement, sulphoaluminate refractory cement, silica powder and vermiculite sand, adding redispersible latex powder, an auxiliary agent and a flame retardant, mixing and stirring, adding volcanic rock, and continuing stirring to obtain the high-strength fireproof mortar;
The mortar comprises the following raw materials, by mass, 100 parts of Portland cement, 115 parts of sulphoaluminate refractory cement, 15 parts of silica powder, 8 parts of redispersible latex powder, 2.5 parts of an auxiliary agent, 100 parts of vermiculite sand, 460 parts of volcanic rock and 40 parts of a flame retardant;
the volcanic rock particle size is 30 meshes, and the stacking density is 500kg/m 3;
The auxiliary agent is a thickening agent, an air entraining agent, a retarder and a water reducing agent, wherein the thickening agent is hydroxypropyl cellulose ether, the air entraining agent is alpha-sodium alkenyl sulfonate, and the retarder is sodium gluconate;
The water reducer is an organosilicon modified polycarboxylate water reducer, and the preparation method comprises the following steps:
mixing 42g of allyl polyoxyethylene ether and 12g of vinyl branched polysiloxane, adding 100mL of mixed solution of deionized water, 56g of acrylic acid and 1g of potassium persulfate, heating to 78 ℃, preserving heat for 5 hours, cooling, dialyzing for 2d by using deionized water, and drying to obtain the organosilicon modified polycarboxylate water reducer;
the flame retardant is composite aluminum hydroxide, and the preparation method comprises the following steps:
(1) Mixing 30g of aluminum hydroxide with 300g of ethanol, adding 8g of (3-mercaptopropyl) trimethoxysilane, preserving heat for 12h at 48 ℃, filtering, washing, drying and grinding to obtain mercaptoaluminum hydroxide;
(2) Mixing 6g of adenosine monophosphate and 40mL of dimethyl sulfoxide, adding 2.2mL of 0.1mol/L hydrochloric acid solution, adding 5mL of glycidyl methacrylate, heating to 90 ℃, preserving heat for 7h, adding 100mL of ethyl acetate, performing suction filtration, washing and drying to obtain a flame retardant monomer containing double bonds;
(3) Mixing 6.2g of vinyl branched polysiloxane, 4.5g of flame-retardant monomer containing double bonds and 12.6g of sulfhydrylation aluminum hydroxide, adding a mixed solution of 0.2g of benzoin dimethyl ether and 80mL of tetrahydrofuran, irradiating for 20min under an ultraviolet lamp with the wavelength of 325nm, performing rotary evaporation, adding 50mL of petroleum ether, filtering, performing rotary evaporation, and drying to obtain composite aluminum hydroxide;
The preparation method of the vinyl branched polysiloxane comprises the following steps of mixing 2.41g of dipropylene glycol and 1.9g of vinyl triethoxysilane under nitrogen atmosphere, adding 0.02g of barium hydroxide, heating to 78 ℃ until the system is clear, heating to 118 ℃ and preserving heat for 12min, continuing to preserve heat for 3h, cooling and filtering to obtain the vinyl branched polysiloxane.
The embodiment 3 is a preparation process of the high-strength fireproof mortar, which comprises the following steps of mixing silicate cement, sulphoaluminate refractory cement, silica powder and vermiculite sand, adding redispersible latex powder, an auxiliary agent and a flame retardant, mixing and stirring, adding volcanic rock, and continuing stirring to obtain the high-strength fireproof mortar;
The mortar comprises 130 parts of silicate cement, 120 parts of sulphoaluminate refractory cement, 25 parts of silica powder, 15 parts of redispersible emulsion powder, 3.9 parts of auxiliary agent, 132 parts of vermiculite sand, 520 parts of volcanic rock and 62 parts of flame retardant;
The volcanic rock particle size is 80 meshes, and the stacking density is 520kg/m 3;
The auxiliary agent is a thickening agent, an air entraining agent, a retarder and a water reducing agent, wherein the thickening agent is hydroxypropyl cellulose ether, the air entraining agent is alpha-sodium alkenyl sulfonate, and the retarder is sodium gluconate;
The water reducer is an organosilicon modified polycarboxylate water reducer, and the preparation method comprises the following steps:
Mixing 42g of allyl polyoxyethylene ether and 12g of vinyl branched polysiloxane, adding 100mL of mixed solution of deionized water, 56g of acrylic acid and 1g of potassium persulfate, heating to 80 ℃, preserving heat for 4.5h, cooling, dialyzing with deionized water for 2d, and drying to obtain an organosilicon modified polycarboxylate water reducer;
the flame retardant is composite aluminum hydroxide, and the preparation method comprises the following steps:
(1) Mixing 30g of aluminum hydroxide with 300g of ethanol, adding 8g of (3-mercaptopropyl) trimethoxysilane, preserving heat for 11h at 50 ℃, filtering, washing, drying and grinding to obtain mercaptoaluminum hydroxide;
(2) Mixing 6g of adenosine monophosphate and 40mL of dimethyl sulfoxide, adding 2.2mL of 0.1mol/L hydrochloric acid solution, adding 5mL of glycidyl methacrylate, heating to 92 ℃, preserving heat for 6.5h, adding 100mL of ethyl acetate, performing suction filtration, washing and drying to obtain a flame-retardant monomer containing double bonds;
(3) Mixing 6.2g of vinyl branched polysiloxane, 4.5g of flame-retardant monomer containing double bonds and 12.6g of sulfhydrylation aluminum hydroxide, adding a mixed solution of 0.2g of benzoin dimethyl ether and 80mL of tetrahydrofuran, irradiating for 25min under an ultraviolet lamp with the wavelength of 325nm, performing rotary evaporation, adding 50mL of petroleum ether, filtering, performing rotary evaporation, and drying to obtain composite aluminum hydroxide;
The preparation method of the vinyl branched polysiloxane comprises the following steps of mixing 2.41g of dipropylene glycol and 1.9g of vinyl triethoxysilane in a nitrogen atmosphere, adding 0.02g of barium hydroxide, heating to 80 ℃ until the system is clear, heating to 120 ℃ and preserving heat for 10min, continuing to preserve heat for 3.5h, cooling and filtering to obtain the vinyl branched polysiloxane.
The embodiment 4 is a preparation process of the high-strength fireproof mortar, which comprises the following steps of mixing silicate cement, sulphoaluminate refractory cement, silica powder and vermiculite sand, adding redispersible latex powder, an auxiliary agent and a flame retardant, mixing and stirring, adding volcanic rock, and continuing stirring to obtain the high-strength fireproof mortar;
The mortar comprises, by mass, 150 parts of Portland cement, 150 parts of sulphoaluminate refractory cement, 30 parts of silica powder, 20 parts of redispersible emulsion powder, 4.8 parts of auxiliary agent, 150 parts of vermiculite sand, 580 parts of volcanic rock and 80 parts of flame retardant;
The volcanic rock particle size is 100 meshes, and the bulk density is 550kg/m 3;
the auxiliary agent is a thickening agent, an air entraining agent, a retarder and a water reducing agent, wherein the thickening agent is hydroxypropyl cellulose ether, the air entraining agent is alpha-sodium alkenyl sulfonate, and the retarder is sodium gluconate;
The water reducer is an organosilicon modified polycarboxylate water reducer, and the preparation method comprises the following steps:
Mixing 42g of allyl polyoxyethylene ether and 12g of vinyl branched polysiloxane, adding 100mL of mixed solution of deionized water, 56g of acrylic acid and 1g of potassium persulfate, heating to 82 ℃, preserving heat for 4 hours, cooling, dialyzing for 2d by using deionized water, and drying to obtain the organosilicon modified polycarboxylate water reducer;
the flame retardant is composite aluminum hydroxide, and the preparation method comprises the following steps:
(1) Mixing 30g of aluminum hydroxide with 300g of ethanol, adding 8g of (3-mercaptopropyl) trimethoxysilane, preserving heat for 10 hours at 52 ℃, filtering, washing, drying and grinding to obtain mercaptoaluminum hydroxide;
(2) Mixing 6g of adenosine monophosphate and 40mL of dimethyl sulfoxide, adding 2.2mL of 0.1mol/L hydrochloric acid solution, adding 5mL of glycidyl methacrylate, heating to 95 ℃, preserving heat for 6h, adding 100mL of ethyl acetate, performing suction filtration, washing and drying to obtain a flame-retardant monomer containing double bonds;
(3) Mixing 6.2g of vinyl branched polysiloxane, 4.5g of flame-retardant monomer containing double bonds and 12.6g of sulfhydrylation aluminum hydroxide, adding a mixed solution of 0.2g of benzoin dimethyl ether and 80mL of tetrahydrofuran, irradiating for 30min under an ultraviolet lamp with the wavelength of 325nm, performing rotary evaporation, adding 50mL of petroleum ether, filtering, performing rotary evaporation, and drying to obtain composite aluminum hydroxide;
The preparation method of the vinyl branched polysiloxane comprises the following steps of mixing 2.41g of dipropylene glycol and 1.9g of vinyl triethoxysilane under nitrogen atmosphere, adding 0.02g of barium hydroxide, heating to 82 ℃ until the system is clear, heating to 122 ℃ and preserving heat for 8min, continuing to preserve heat for 4h, cooling and filtering to obtain the vinyl branched polysiloxane.
Comparative example 1 with example 1 as the control group, no vermiculite sand was added, and the other procedures were normal.
Comparative example 2 Using example 3 as a control, the composite aluminum hydroxide was replaced with thiolated aluminum hydroxide, and the other procedures were normal.
Comparative example 3 Using example 3 as a control group, the silicone modified polycarboxylate water reducer was replaced with the polycarboxylate water reducer, and the other procedures were normal.
Comparative example 4 Using example 3 as a control, no vinyl branched polysiloxane was prepared and the other procedures were normal.
Raw material source (by way of example only):
Silicate cement P.O525:Skyline limited, sulphoaluminate refractory cement S.SACC525: gongyi, sanand refractory limited, silica powder (96 grade) Hebei Yi Rui alloy welding material limited, bdelloving sand (10-20 mesh) Lingshou A.D. mineral powder mill, redispersible emulsion powder 5044N, guangdong Lap technology limited, hydroxypropyl cellulose ether H100, shandong Yiteng cellulose limited, alpha-alkenyl sodium sulfonate AOS, zhejiang Zan technology limited, sodium gluconate, jinan Guangxi chemical technology limited, polycarboxylate water reducer P622, suzhou make the country prosperous chemical building material limited, aluminum hydroxide SS-AL04, ulagi Jikang new material limited, adenosine monophosphate (98 percent) to Chamomerization Chamom chemical limited, benzoin dimethyl ether S45044, shanghai Ye biological limited, allyl polyoxyethylene ether A303301, acrylic acid A103526, (3-mercaptopropyl silane M100619, dimethyl sulfoxide F, methyl sulfoxide F, 35D 35, 35 ethyl alcohol 35, 35D, 35 ethyl alcohol, 35, and ethylene glycol.
Performance test the mortar prepared in examples and comparative examples was subjected to performance test:
when performance tests are carried out, the mass ratio of the mortar to the purified water in the examples and the comparative examples is 1:5.8;
the adhesive strength and the compressive strength are detected by referring to a JGJ70-2009 building mortar basic performance test method, the thermal conductivity is measured by referring to a GB/T10297 nonmetal solid material thermal conductivity coefficient, the fire resistance is measured by referring to a GB 14007-2018 steel structure fireproof paint fire resistance test method, and the results are shown in the following table 1;
TABLE 1
The invention provides high-strength fireproof mortar and a preparation process thereof, and the high-strength fireproof mortar is high in strength and excellent in cohesiveness, fireproof heat insulation and corrosion resistance through component and proportion design.
By comparing the embodiment 1 with the comparative embodiment 1, the mortar has the advantages of high strength, low density, low thermal conductivity and the like by adding the vermiculite sand as the fireproof material into the mortar.
In order to improve the fireproof performance of mortar, aluminum hydroxide is used as an environment-friendly flame retardant, the aluminum hydroxide is modified, the surface of the aluminum hydroxide is thiolated by (3-mercaptopropyl) trimethoxysilane, and then is subjected to light-point impact by mercapto-double bond, and a flame-retardant monomer containing double bond and vinyl branched polysiloxane are introduced to the surface of the aluminum hydroxide, so that the flame-retardant monomer containing double bond plays a role in synergistic flame retardance and fire prevention under the action of the flame-retardant monomer containing double bond and the vinyl branched polysiloxane, wherein the flame-retardant monomer containing double bond is a flame-retardant monomer prepared by modifying an intumescent micromolecular flame retardant adenosine monophosphate by adopting glycidyl methacrylate, and the vinyl branched polysiloxane is dipropylene glycol and vinyl triethoxysilane to synthesize a polysiloxane containing a large amount of Si-O bonds and double bonds.
By comparing example 3 with comparative example 3 and comparative example 4, the invention uses the allyl polyoxyethylene ether as the raw material of the high-efficiency polycarboxylate water reducer as the main chain, and the vinyl branched polysiloxane with strong grafting reaction activity and the acrylic acid with strong hydrophilicity are used for preparing the organosilicon modified polycarboxylate water reducer with strong hydrophilicity, high reaction activity and high water reducing effect, thereby improving the bonding strength and corrosion resistance of the mortar and prolonging the service life of the mortar.
The foregoing description is only exemplary embodiments of the present invention and is not intended to limit the scope of the invention, and all equivalent structural changes made by the present invention or direct/indirect application in other related technical fields are included in the scope of the present invention.

Claims (8)

1. The high-strength fireproof mortar is characterized by comprising, by mass, 100-150 parts of Portland cement, 115-150 parts of sulphoaluminate refractory cement, 15-30 parts of silica powder, 8-20 parts of redispersible emulsion powder, 2.5-4.8 parts of auxiliary agent, 100-150 parts of vermiculite sand, 460-580 parts of volcanic rock and 40-80 parts of flame retardant;
the flame retardant is composite aluminum hydroxide, and the preparation method comprises the following steps:
(1) Mixing aluminum hydroxide and ethanol, adding (3-mercaptopropyl) trimethoxy silane, preserving heat for 10-12h at 48-52 ℃, filtering, washing, drying and grinding to obtain mercaptoaluminum hydroxide;
(2) Mixing adenosine monophosphate and dimethyl sulfoxide, adding hydrochloric acid, adding glycidyl methacrylate, heating to 90-95 ℃ and preserving heat for 6-7h, adding ethyl acetate, filtering, washing and drying to obtain a flame-retardant monomer containing double bonds;
(3) Mixing vinyl branched polysiloxane, a double bond-containing flame-retardant monomer and sulfhydrylated aluminum hydroxide, adding a mixed solution of benzoin dimethyl ether and tetrahydrofuran, irradiating for 20-30min under an ultraviolet lamp with the wavelength of 325nm, performing rotary evaporation, adding petroleum ether, filtering, performing rotary evaporation, and drying to obtain the composite aluminum hydroxide.
2. The high-strength fireproof mortar according to claim 1, wherein the volcanic rock has a particle size of 30-100 meshes and a bulk density of 500-550kg/m 3.
3. The high-strength fireproof mortar according to claim 1, wherein the auxiliary agent is a thickener, an air entraining agent, a retarder and a water reducing agent, and the high-strength fireproof mortar is obtained by compounding the components in a mass ratio of (1.8-3) (0.1-0.4) (0.5-1).
4. The high-strength fireproof mortar according to claim 3, wherein the thickener is hydroxypropyl cellulose ether, the air entraining agent is alpha-sodium alkenyl sulfonate, and the retarder is sodium gluconate.
5. A high strength fire protection mortar according to claim 3, wherein the water reducing agent is a polycarboxylate water reducing agent.
6. A high strength fire protection mortar according to claim 3, wherein the water reducer is an organosilicon modified polycarboxylate water reducer, and the preparation comprises the following steps:
Mixing allyl polyoxyethylene ether and vinyl branched polysiloxane, adding a mixed solution of deionized water, acrylic acid and potassium persulfate, heating to 78-82 ℃, preserving heat for 4-5h, cooling, dialyzing with deionized water for 2d, and drying to obtain the organosilicon modified polycarboxylate water reducer.
7. The high-strength fireproof mortar according to claim 1, wherein the preparation of the vinyl branched polysiloxane comprises the following steps of mixing dipropylene glycol and vinyl triethoxysilane in a nitrogen atmosphere, adding barium hydroxide, heating to 78-82 ℃ until the system is clear, heating to 118-122 ℃ and preserving heat for 8-12min, continuing to preserve heat for 3-4h, cooling and filtering to obtain the vinyl branched polysiloxane.
8. The process for preparing the high-strength fireproof mortar according to any one of claims 1 to 7, which is characterized by comprising the following steps of mixing silicate cement, sulphoaluminate refractory cement, silica fume and vermiculite sand, adding redispersible latex powder, an auxiliary agent and a flame retardant, mixing and stirring, adding volcanic rock, and continuing stirring to obtain the high-strength fireproof mortar.
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CN110229338A (en) * 2019-04-28 2019-09-13 武汉理工大学 A kind of hyperbranched polyorganosiloxane and its preparation method and application
CN110317021A (en) * 2019-07-09 2019-10-11 中国十七冶集团有限公司 It is a kind of heat preservation and fire resisting integration jet printing type mortar
CN111943604A (en) * 2020-08-25 2020-11-17 中交路桥建设有限公司 Prestressed duct grouting material

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