CN114835446A - Heat-insulation ceramsite concrete material and preparation method thereof - Google Patents

Heat-insulation ceramsite concrete material and preparation method thereof Download PDF

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CN114835446A
CN114835446A CN202210620534.9A CN202210620534A CN114835446A CN 114835446 A CN114835446 A CN 114835446A CN 202210620534 A CN202210620534 A CN 202210620534A CN 114835446 A CN114835446 A CN 114835446A
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ceramsite
mass
ceramsite concrete
mixing
composite
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CN114835446B (en
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张皓
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Xi'an Gao Ke Xin Da Concrete Co ltd
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Abstract

The invention discloses a heat-insulation ceramsite concrete material and a preparation method thereof, and relates to the technical field of concrete. Firstly, mixing tetraphenyl silicate and trimethyl aluminate for primary calcination to form silica aerogel, alumina and carbon nanowires, and preparing to obtain composite ceramsite; mixing phosphorus pentachloride, composite ceramsite, light sand, cement, quicklime and water to prepare a ceramsite concrete base material; finally, performing secondary calcination by utilizing polyacrylic benzoic acid formamide to form a polypropylene network taking cyclophosphazene as a center, calcining part of the polypropylene network to form a compact carbon layer and nitrogen, and reducing aluminum formed by alumina by the compact carbon layer to react with the nitrogen to form aluminum nitride grains to prepare the heat-insulating ceramsite concrete material; the heat-insulating ceramsite concrete material prepared by the method has good heat-insulating property, flame retardant property, anti-cracking property and toughness.

Description

Heat-insulation ceramsite concrete material and preparation method thereof
Technical Field
The invention relates to the technical field of concrete, in particular to a heat-insulation ceramsite concrete material and a preparation method thereof.
Background
Concrete is a general name of composite materials which are prepared by mixing gel materials, aggregates and water according to a proper proportion and then are hardened for a certain time, and is the artificial civil engineering and construction material with the largest usage amount in the world. The common gel material is cement, and the common aggregate is stone and sand. The concrete has high hardness, wide raw material sources and low cost, and is widely used for buildings, roads, military engineering, nuclear power plants and other structures.
Along with the development of society and the rapid improvement of living standard, the requirements of people on buildings are improved, and concrete gradually develops towards the light weight heat preservation direction, wherein, ceramsite concrete is concrete prepared by replacing stones with ceramsite as concrete aggregate, and is light weight and heat preservation due to loose and porous structure, thus, the ceramsite concrete is also separated from various concrete materials at present and is widely applied to the field of buildings.
However, the ceramsite concrete in the prior art often has the phenomena of cracking, aging, powder removal and the like in the daily use process, is not high enough in fire resistance, has more potential safety hazards, and greatly influences the application of the ceramsite concrete. The invention focuses on the current situation and solves the problems by preparing an insulating ceramsite concrete material.
Disclosure of Invention
The invention aims to provide a heat-insulating ceramsite concrete material and a preparation method thereof, which aim to solve the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
the heat-insulating ceramsite concrete material is prepared by carrying out secondary calcination on a ceramsite concrete base material by utilizing polyacrylic benzoic acid formamide.
Furthermore, the ceramsite concrete base material is prepared by mixing phosphorus pentachloride, composite ceramsite, light sand, quicklime, cement and water.
Further, the composite ceramsite is prepared by mixing tetraphenyl silicate and trimethyl aluminate and then calcining for one time.
The preparation method of the heat-insulation ceramsite concrete material comprises the following preparation steps:
(1) mixing composite ceramsite, light sand, quicklime, cement and 60-80 ℃ deionized water according to a mass ratio of 1: 0.3: 0.14: 0.7: 1.1-1: 0.5: 0.16: 0.9: 1.3, mixing, shearing for 4-6 h at 4500-5000 r/min, adding phosphorus pentachloride with the mass 0.6-0.8 time of that of the composite ceramsite, shearing for 4-6 h, pouring into a mold at 48-52 ℃ for fixation for 4-6 h, and drying at 80-90 ℃ for 23-25 h to obtain a ceramsite concrete base material;
(2) placing a ceramsite concrete base material into a closed container with the pressure of 3-5 MPa at room temperature under the protection of argon, pouring polyacrylic benzoic acid formamide with the mass of 0.4-0.6 time of that of the ceramsite concrete base material, dropwise adding 30% by mass of sodium hydroxide solution at the rate of 60 drops/min, adjusting the pH value to 9, standing for 1-3 h, and then, mixing the raw materials in a mass ratio of 1: 8-1: 12, adding zinc oxide and pyridine, wherein the mass of the zinc oxide is 0.01-0.016 times of that of the ceramsite concrete base material, performing ultrasonic treatment for 10-20 min at 30-40 kHz, performing microwave treatment for 15-25 min under the microwave conditions of 2400-2500 MHz and 700-900W, adding dimethyl sulfate which is 0.01-0.03 times of that of the ceramsite concrete base material, continuing performing microwave treatment for 30-50 min, demolding, putting the mixture into a reaction kettle with the pressure of 0.7-0.9 MPa, heating to 660-680 ℃ at 9-11 ℃/min, keeping the temperature for 2-6 h, heating to 1200-1400 ℃, and keeping the temperature for 4-10 h to prepare the ceramsite concrete material.
Further, the preparation method of the composite ceramsite in the step (1) comprises the following steps: the composite sol is placed in a refrigerator at the temperature of-4 to-2 ℃ for freezing for 47-49 hours, dried for 47-49 hours at the temperature of 10-20 Pa and-50 to-40 ℃, washed for 2-4 times by absolute ethyl alcohol, placed in a drying oven at the temperature of 10-20 Pa and 19-21 ℃ for drying for 1-3 hours, soaked in a nickel nitrate solution with the mass fraction of 10% and the mass being 0.2-0.3 time of that of the composite sol for 10-20 hours, fished out and placed in a reaction kettle at the pressure of 0.7-0.9 MPa, heated to 690-710 ℃ at the speed of 9-11 ℃/min, insulated for 1-3 hours, heated to 1300-1500 ℃ after heat preservation for 1-3 hours, insulated for 1-3 hours, naturally cooled to the normal temperature, then washed for 3-5 times by absolute ethyl alcohol, and placed in the drying oven at the temperature of 30-40 ℃ for drying for 1-3 hours, and the composite ceramsite is prepared.
Further, the preparation method of the composite sol comprises the following steps: under the conditions of 80-90 ℃ and argon protection, trimethyl aluminate and deionized water are mixed according to the mass ratio of 1: 7-1: 9, stirring for 1-3 hours at 400-600 r/min, dripping a nitric acid solution with the mass fraction of 11-13% and the mass of 0.2-0.3 times of that of trimethyl aluminate at 40-60 drops/min, continuously stirring for 1-3 hours, adding silver with the mass of 0.01-0.03 times of that of trimethyl aluminate, heating to 500-560 ℃ at 9-11 ℃/min, keeping the temperature for 8-10 hours, cooling to 24-26 ℃ at 9-11 ℃/min, adding tetraphenyl silicate with the mass of 2-4 times of that of trimethyl aluminate, continuously dripping ethanol with the mass of 8-16 times of that of trimethyl aluminate, continuously stirring for 2-4 hours at 60-80 ℃, adding ammonium hydroxide with the mass of 0.08-0.16 times of that of trimethyl aluminate, continuously stirring for 10-20 minutes, heating to 65-85 ℃ at 2-4 ℃/min, continuously stirring for 10-20 minutes, continuously heating to 95-105 ℃, stirring for 60-80 minutes at 600-800 r/min, and preparing the composite sol.
Further, the light sand in the step (1) has fineness modulus of 1.6 and apparent density of 2870kg/m 3 The natural river sand.
Further, the preparation method of the polyacrylic benzoic acid formamide in the step (2) comprises the following steps: under the conditions of room temperature and argon protection, the method comprises the following steps of mixing propenylbenzoic acid and formamide according to a mass ratio of 1: 0.6-1: 0.8, stirring for 20-30 min at 400-600 r/min, then adding nano titanium dioxide which is 0.06-0.08 times of the mass of the acrylic benzoic acid, heating to 80-100 ℃ at 9-10 ℃/min, and continuously stirring for 2-4 h to prepare the polyacrylic benzoic acid formamide.
Further, the preparation method of the polyacrylic benzoic acid comprises the following steps: at room temperature and under the protection of argon, mixing chlorinated polypropylene and benzoic acid according to a mass ratio of 1: 3-1: 5, mixing, stirring for 10-20 min at 400-600 r/min, adding aluminum trichloride of which the mass is 0.01-0.03 time that of chlorinated polypropylene, cooling to 0-4 ℃ at 2-4 ℃/min, stirring for 7-9 h at 600-800 r/min, and thus obtaining the polyacrylic benzoic acid.
Furthermore, the molecular weight of the chlorinated polypropylene is 1000-3000.
Compared with the prior art, the invention has the following beneficial effects:
when the heat-preservation ceramsite concrete material is prepared, tetraphenyl silicate and trimethyl aluminate are mixed and calcined for the first time to prepare the composite ceramsite; mixing phosphorus pentachloride, composite ceramsite, light sand, cement, quicklime and water to prepare a ceramsite concrete base material; and finally, carrying out secondary calcination on the ceramsite concrete base material by utilizing the polyacrylic benzoic acid formamide to prepare the heat-insulating ceramsite concrete material.
Firstly, tetraphenyl silicate and trimethyl aluminate are hydrolyzed, phenol and methanol are removed, and then the reaction and crosslinking are carried out to form silica aerogel and alumina, so that the heat preservation performance of the composite ceramsite is enhanced; the methanol is oxidized to form formaldehyde, the formaldehyde reacts with phenol to form a phenolic network, a large number of carbon nanowires are formed in the composite ceramsite after the phenolic network is carbonized, and when microcracks and residual stress are generated, the cracks can be nailed together, so that the toughness of the composite ceramsite is enhanced.
Secondly, hydrolyzing part of phosphorus pentachloride to form phosphoric acid and hydrogen chloride, activating the ceramsite concrete base material by the phosphoric acid, forming a large number of free radicals such as hydroxyl groups in the ceramsite concrete base material, hydrolyzing the polyacrylic benzoic acid formamide to form formamide and polyacrylic benzoic acid, decomposing the formamide to react with the hydrogen chloride to form ammonium chloride, and reacting the ammonium chloride with part of the phosphorus pentachloride to form hexachlorocyclophosphazene, so that the flame retardant property of the heat-insulating ceramsite concrete material is enhanced; carboxyl on the polypropylene benzoic acid reacts with hydroxyl in the ceramsite concrete base material for crosslinking, hexachlorocyclophosphazene reacts with benzene rings on the polypropylene benzoic acid for crosslinking to form a polypropylene network taking the cyclophosphazene as the center, when the ceramsite concrete base material is calcined, the cyclophosphazene in part of the polypropylene network is taken as an acid source and a gas source, the polypropylene benzoic acid is taken as a carbon source, a compact carbon layer and a large amount of nitrogen are formed in the ceramsite concrete base material, aluminum oxide in the composite ceramsite is reduced into aluminum by the carbon layer, part of molten aluminum flows out of the composite ceramsite and reacts with the nitrogen to form aluminum nitride grains, the composite ceramsite and the cement base material are firmly embedded together, and the anti-cracking performance of the heat-preservation ceramsite concrete material is enhanced.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to more clearly illustrate the method provided by the invention, the following examples are used for detailed description, and the method for testing each index of the thermal insulation ceramsite concrete material prepared in the following examples is as follows:
thermal insulation performance: the thermal conductivity coefficient of the thermal insulation ceramsite concrete materials prepared in the same mass examples and comparative examples is measured according to the GB/T10295 standard method to measure the thermal insulation performance.
Flame retardant property: the flame retardance of the heat-insulating ceramsite concrete material prepared by the same mass of the examples and the comparative example is measured by testing the oxygen index according to the GB/T29051 standard method.
Anti-cracking performance: the thermal insulation ceramsite concrete material prepared by the embodiment and the comparative example with the same length and width is used for measuring the cracking resistance by measuring the splitting tensile strength according to the GB/T50081 standard method.
Toughness: the fracture toughness of the ultra-fine grained titanium-based high-plastic ceramic material prepared by the embodiment and the comparative example with the same length and width is tested according to ASTMC 1421.
Example 1
The preparation method of the heat-insulation ceramsite concrete material comprises the following preparation steps:
(1) under the conditions of 80 ℃ and argon protection, trimethyl aluminate and deionized water are mixed according to the mass ratio of 1: 7, mixing, stirring for 1h at 400r/min, dropwise adding a nitric acid solution with the mass fraction of 11% and the mass of 0.2 time of trimethyl aluminate at 40 drops/min, continuously stirring for 1h, adding silver with the mass of 0.01 time of trimethyl aluminate, heating to 500 ℃ at 9 ℃/min, preserving heat for 8h, cooling to 24 ℃ at 9 ℃/min, adding tetraphenyl silicate with the mass of 2 times of trimethyl aluminate, continuously dropwise adding ethanol with the mass of 8 times of trimethyl aluminate, continuously stirring for 2h at 60 ℃, adding ammonium hydroxide with the mass of 0.08 time of trimethyl aluminate, continuously stirring for 10min, heating to 65 ℃ at 2 ℃/min, continuously stirring for 10min, continuously heating to 95 ℃, and stirring for 60min at 600r/min to prepare a composite sol; freezing the composite sol in a refrigerator at the temperature of-4 ℃ for 47h, drying at the temperature of 10Pa and-50 ℃ for 47h, washing with absolute ethyl alcohol for 2 times, drying in a drying oven at the temperature of 10Pa and 19 ℃ for 1h, soaking in a nickel nitrate solution with the mass fraction of 10 percent which is 0.2 time of the mass of the composite sol for 10h, taking out, putting in a reaction kettle at the pressure of 0.7MPa, heating to 690 ℃ at the speed of 9 ℃/min, preserving heat for 1h, heating to 1300 ℃, preserving heat for 1h, naturally cooling to the normal temperature, washing with absolute ethyl alcohol for 3 times, and drying in a drying oven at the temperature of 30 ℃ for 1h to prepare the composite ceramsite;
(2) mixing composite ceramsite, light sand, quicklime, cement and 60 ℃ deionized water according to a mass ratio of 1: 0.3: 0.14: 0.7: 1.1, mixing, shearing for 4h at 4500r/min, adding phosphorus pentachloride with the mass 0.6 times of that of the composite ceramsite, shearing for 4h, pouring into a mold at 48 ℃ for fixing for 4h, and drying at 80 ℃ for 23h to obtain a ceramsite concrete base material;
(3) at room temperature and under the protection of argon, mixing chlorinated polypropylene with molecular weight of 1000 and benzoic acid according to a mass ratio of 1: 3, mixing, stirring for 10min at 400r/min, adding aluminum trichloride of which the mass is 0.01 time that of chlorinated polypropylene, cooling to 0 ℃ at 2 ℃/min, stirring for 7h at 600r/min, and preparing to obtain polyacrylic benzoic acid; under the conditions of room temperature and argon protection, the method comprises the following steps of mixing propenylbenzoic acid and formamide according to a mass ratio of 1: 0.6, stirring at 400r/min for 20min, then adding nano titanium dioxide with the mass of 0.06 time that of the acrylic benzoic acid, heating to 80 ℃ at 9 ℃/min, and continuously stirring for 2h to prepare the polyacrylic benzoic acid formamide; placing a ceramsite concrete base material into a closed container with the pressure of 3MPa at room temperature under the protection of argon, pouring polyacrylic benzoic acid formamide with the mass of 0.4 time that of the ceramsite concrete base material, dropwise adding 30% by mass of sodium hydroxide solution at the rate of 60 drops/min, adjusting the pH value to 9, standing for 1h, and then, mixing the components in a mass ratio of 1: 8, adding zinc oxide and pyridine, wherein the mass of the zinc oxide is 0.01 time of that of the ceramsite concrete base material, carrying out ultrasonic treatment for 10min at 30kHz, carrying out microwave treatment for 15min under the microwave conditions of 2400MHz and 700W, adding dimethyl sulfate which is 0.01 time of that of the ceramsite concrete base material, continuing the microwave treatment for 30min, demoulding, putting the mixture into a 0.7MPa reaction kettle, heating to 660 ℃ at 9 ℃/min, carrying out heat preservation for 2h, heating to 1200 ℃, and carrying out heat preservation for 4h to prepare the ceramsite concrete material.
Example 2
The preparation method of the heat-insulation ceramsite concrete material comprises the following preparation steps:
(1) under the conditions of 85 ℃ and argon protection, trimethyl aluminate and deionized water are mixed according to the mass ratio of 1: 8, mixing, stirring for 2h at 500r/min, dropwise adding a nitric acid solution with the mass fraction of 12% and the mass of 0.25 time of trimethyl aluminate at 50 drops/min, continuing to stir for 2h, adding silver with the mass of 0.02 time of trimethyl aluminate, heating to 530 ℃ at 10 ℃/min, keeping the temperature for 9h, cooling to 25 ℃ at 10 ℃/min, adding tetraphenyl silicate with the mass of 3 times of trimethyl aluminate, continuing to dropwise add ethanol with the mass of 12 times of trimethyl aluminate, continuing to stir for 3h at 70 ℃, adding ammonium hydroxide with the mass of 0.12 time of trimethyl aluminate, continuing to stir for 15min, heating to 75 ℃ at 3 ℃/min, continuing to stir for 15min, continuing to heat to 100 ℃, and stirring for 70min at 700r/min to prepare a composite sol; putting the composite sol into a refrigerator at the temperature of-3 ℃ for freezing for 48h, drying for 48h at the temperature of 15Pa and-45 ℃, washing for 3 times by using absolute ethyl alcohol, putting the composite sol into a drying oven at the temperature of 15Pa and 20 ℃ for drying for 2h, then soaking the composite sol into a nickel nitrate solution with the mass fraction of 10 percent which is 0.25 time of the mass of the composite sol for 15h, fishing out the composite sol, putting the composite sol into a reaction kettle at the pressure of 0.8MPa, heating to 700 ℃ at the speed of 10 ℃/min, preserving heat for 2h, heating to 1400 ℃, preserving heat for 2h, naturally cooling to the normal temperature, then washing for 4 times by using absolute ethyl alcohol, putting the composite sol into a drying oven at the temperature of 35 ℃ for drying for 2h, and preparing the composite ceramsite;
(2) mixing composite ceramsite, light sand, quicklime, cement and 70 ℃ deionized water according to a mass ratio of 1: 0.4: 0.15: 0.8: 1.2, mixing, shearing for 5h at 4750r/min, adding phosphorus pentachloride with the mass of 0.7 time of that of the composite ceramsite, shearing for 5h, pouring into a mold at 50 ℃ for fixing for 5h, and drying at 85 ℃ for 24h to obtain a ceramsite concrete base material;
(3) at room temperature and under the protection of argon, mixing chlorinated polypropylene with molecular weight of 2000 and benzoic acid according to a mass ratio of 1: 4, mixing, stirring for 15min at 500r/min, adding aluminum trichloride of which the mass is 0.02 time that of chlorinated polypropylene, cooling to 2 ℃ at 3 ℃/min, stirring for 8h at 700r/min, and preparing to obtain polyacrylic benzoic acid; under the conditions of room temperature and argon protection, the method comprises the following steps of mixing propenylbenzoic acid and formamide according to a mass ratio of 1: 0.7, stirring at 500r/min for 25min, then adding nano titanium dioxide with the mass of 0.07 time of that of the acrylic benzoic acid, heating to 90 ℃ at 9.5 ℃/min, and continuously stirring for 3h to prepare the polyacrylic benzoic acid formamide; placing a ceramsite concrete base material into a 4MPa closed container at room temperature under the protection of argon, pouring polyacrylic benzoic acid formamide with the mass of 0.5 time of that of the ceramsite concrete base material, dropwise adding a 30% sodium hydroxide solution at a rate of 60 drops/min, adjusting the pH value to 9, standing for 2 hours, and then mixing the components in a mass ratio of 1: 10, adding zinc oxide and pyridine, wherein the mass of the zinc oxide is 0.013 times of that of the ceramsite concrete base material, carrying out ultrasonic treatment for 15min at 35kHz, carrying out microwave treatment for 20min under the microwave conditions of 2450MHz and 800W, adding dimethyl sulfate which is 0.02 times of that of the ceramsite concrete base material, continuing the microwave treatment for 40min, demoulding, putting the mixture into a 0.8MPa reaction kettle, heating to 670 ℃ at the speed of 10 ℃/min, carrying out heat preservation for 4h, heating to 1300 ℃, and carrying out heat preservation for 7h to prepare the ceramsite concrete material.
Example 3
The preparation method of the heat-insulation ceramsite concrete material comprises the following preparation steps:
(1) under the conditions of 90 ℃ and argon protection, trimethyl aluminate and deionized water are mixed according to the mass ratio of 1: 9, mixing, stirring for 3 hours at 600r/min, dropwise adding a nitric acid solution with the mass fraction of 13% and the mass of 0.3 time of that of trimethyl aluminate at 60 drops/min, continuing to stir for 3 hours, adding silver with the mass of 0.03 time of that of trimethyl aluminate, heating to 560 ℃ at 11 ℃/min, preserving heat for 10 hours, cooling to 26 ℃ at 11 ℃/min, adding tetraphenyl silicate with the mass of 4 times of that of trimethyl aluminate, continuing to dropwise add ethanol with the mass of 16 times of that of trimethyl aluminate, continuing to stir for 4 hours at 80 ℃, adding ammonium hydroxide with the mass of 0.16 time of trimethyl aluminate, continuing to stir for 20 minutes, heating to 85 ℃ at 4 ℃/min, continuing to stir for 20 minutes, continuing to heat to 105 ℃, and stirring for 80 minutes at 800r/min to prepare the composite sol; freezing the composite sol in a refrigerator at the temperature of-2 ℃ for 49h, drying at the temperature of 20Pa and-40 ℃ for 49h, washing with absolute ethyl alcohol for 4 times, drying in a baking oven at the temperature of 20Pa and 21 ℃ for 3h, soaking in a nickel nitrate solution with the mass fraction of 10 percent which is 0.3 time of the mass of the composite sol for 20h, fishing out, putting in a reaction kettle at the pressure of 0.9MPa, heating to 710 ℃ at the speed of 11 ℃/min, preserving heat for 3h, heating to 1500 ℃, preserving heat for 3h, naturally cooling to normal temperature, washing with absolute ethyl alcohol for 5 times, and drying in a baking oven at the temperature of 40 ℃ for 3h to prepare the composite ceramsite;
(2) mixing composite ceramsite, light sand, quicklime, cement and 80 ℃ deionized water according to a mass ratio of 1: 0.5: 0.16: 0.9: 1.3, mixing, shearing for 6h at 5000r/min, adding phosphorus pentachloride with the mass of 0.8 time of that of the composite ceramsite, shearing for 6h, pouring into a mold at 52 ℃ for fixation for 6h, and drying at 90 ℃ for 25h to obtain a ceramsite concrete base material;
(3) at room temperature and under the protection of argon, chlorinated polypropylene with the molecular weight of 3000 and benzoic acid are mixed according to the mass ratio of 1: 5, mixing, stirring at 600r/min for 20min, adding aluminum trichloride of which the mass is 0.03 time that of chlorinated polypropylene, cooling to 4 ℃ at 4 ℃/min, stirring at 800r/min for 9h, and preparing to obtain polyacrylic benzoic acid; under the conditions of room temperature and argon protection, the method comprises the following steps of mixing propenylbenzoic acid and formamide according to a mass ratio of 1: 0.8, stirring at 600r/min for 30min, then adding nano titanium dioxide with the mass of 0.08 time that of the acrylic benzoic acid, heating to 100 ℃ at the speed of 10 ℃/min, and continuously stirring for 4h to prepare the polyacrylic benzoic acid formamide; placing the ceramsite concrete base material into a 5MPa closed container under the conditions of room temperature and argon protection, pouring polyacrylic benzoic acid formamide with the mass of 0.6 time of that of the ceramsite concrete base material, dropwise adding 30% sodium hydroxide solution with the mass fraction of 60 drops/min, adjusting the pH value to 9, standing for 3h, and then, mixing the raw materials according to the mass ratio of 1: 12 adding zinc oxide and pyridine, wherein the mass of the zinc oxide is 0.016 times of that of the ceramsite concrete base material, carrying out ultrasonic treatment for 20min at 40kHz, carrying out microwave treatment for 25min under the microwave conditions of 2500MHz and 900W, adding dimethyl sulfate which is 0.03 times of that of the ceramsite concrete base material, continuing the microwave treatment for 50min, demoulding, putting the mixture into a 0.9MPa reaction kettle, heating to 680 ℃ at 11 ℃/min, carrying out heat preservation for 6h, heating to 1400 ℃, and carrying out heat preservation for 10h to prepare the ceramsite concrete material.
Comparative example 1
Comparative example 1 differs from example 2 only in step (1), step (1) being modified: under the conditions of 85 ℃ and argon protection, trimethyl aluminate and deionized water are mixed according to the mass ratio of 1: 8, mixing, stirring for 2h at 500r/min, dropwise adding a nitric acid solution with the mass fraction of 12% and the mass of 0.25 time of trimethyl aluminate at 50 drops/min, continuing to stir for 2h, adding silver with the mass of 0.02 time of trimethyl aluminate, heating to 530 ℃ at 10 ℃/min, keeping the temperature for 9h, cooling to 25 ℃ at 10 ℃/min, continuing to dropwise add ethanol with the mass of 12 times of trimethyl aluminate, continuing to stir for 3h at 70 ℃, adding ammonium hydroxide with the mass of 0.12 time of trimethyl aluminate, continuing to stir for 15min, heating to 75 ℃ at 3 ℃/min, continuing to stir for 15min, continuing to heat to 100 ℃, and stirring for 70min at 700r/min to prepare a composite sol; the composite sol is put into a refrigerator with the temperature of minus 3 ℃ for freezing for 48h, dried for 48h at the temperature of 15Pa and minus 45 ℃, washed for 3 times by absolute ethyl alcohol, put into a drying oven with the temperature of 15Pa and 20 ℃ for drying for 2h, then soaked in a nickel nitrate solution with the mass fraction of 10 percent which is 0.25 time of the mass of the composite sol for 15h, taken out and put into a reaction kettle with the pressure of 0.8MPa, heated to 700 ℃ at the speed of 10 ℃/min, kept warm for 2h, heated to 1400 ℃, kept warm for 2h, naturally cooled to the normal temperature, washed for 4 times by absolute ethyl alcohol, put into a drying oven with the temperature of 35 ℃ for drying for 2h, and the composite ceramsite is prepared. The rest of the preparation steps are the same as example 2.
Comparative example 2
Comparative example 2 differs from example 2 only in step (1), step (1) being modified: at the temperature of 25 ℃, tetraphenyl silicate and ethanol are mixed according to the mass ratio of 1: 4, stirring for 25min at 500r/min, then dropwise adding a nitric acid solution with the mass fraction of 12% and 0.25 time of the mass of tetraphenyl silicate at 50 drops/min, continuously stirring for 3h at 85 ℃, and naturally cooling to room temperature to prepare composite sol; the composite sol is put into a refrigerator with the temperature of minus 3 ℃ for freezing for 48h, dried for 48h at the temperature of 15Pa and minus 45 ℃, washed for 3 times by absolute ethyl alcohol, put into a drying oven with the temperature of 15Pa and 20 ℃ for drying for 2h, then soaked in a nickel nitrate solution with the mass fraction of 10 percent which is 0.25 time of the mass of the composite sol for 15h, taken out and put into a reaction kettle with the pressure of 0.8MPa, heated to 700 ℃ at the speed of 10 ℃/min, kept warm for 2h, heated to 1400 ℃, kept warm for 2h, naturally cooled to the normal temperature, washed for 4 times by absolute ethyl alcohol, put into a drying oven with the temperature of 35 ℃ for drying for 2h, and the composite ceramsite is prepared. The rest of the preparation steps are the same as example 2.
Comparative example 3
The preparation method of the heat-insulation ceramsite concrete material comprises the following preparation steps:
(1) mixing shale ceramsite, light sand, quicklime, cement and 70 ℃ deionized water according to a mass ratio of 1: 0.4: 0.15: 0.8: 1.2, mixing, shearing for 5 hours at 4750r/min, adding phosphorus pentachloride with the mass of 0.7 time of that of shale ceramsite, shearing for 5 hours, pouring the mixture into a mold at 50 ℃ for fixing for 5 hours, and drying at 85 ℃ for 24 hours to obtain a ceramsite concrete base material;
(2) at room temperature and under the protection of argon, mixing chlorinated polypropylene with molecular weight of 2000 and benzoic acid according to a mass ratio of 1: 4, mixing, stirring for 15min at 500r/min, adding aluminum trichloride of which the mass is 0.02 time that of chlorinated polypropylene, cooling to 2 ℃ at 3 ℃/min, stirring for 8h at 700r/min, and preparing to obtain polyacrylic benzoic acid; under the conditions of room temperature and argon protection, the method comprises the following steps of mixing propenylbenzoic acid and formamide according to a mass ratio of 1: 0.7, stirring at 500r/min for 25min, then adding nano titanium dioxide with the mass of 0.07 time of that of the acrylic benzoic acid, heating to 90 ℃ at 9.5 ℃/min, and continuously stirring for 3h to prepare the polyacrylic benzoic acid formamide; placing a ceramsite concrete base material into a 4MPa closed container at room temperature under the protection of argon, pouring polyacrylic benzoic acid formamide with the mass of 0.5 time of that of the ceramsite concrete base material, dropwise adding a 30% sodium hydroxide solution at a rate of 60 drops/min, adjusting the pH value to 9, standing for 2 hours, and then mixing the components in a mass ratio of 1: 10, adding zinc oxide and pyridine, wherein the mass of the zinc oxide is 0.013 times of that of the ceramsite concrete base material, carrying out ultrasonic treatment for 15min at 35kHz, carrying out microwave treatment for 20min under the microwave conditions of 2450MHz and 800W, adding dimethyl sulfate which is 0.02 times of that of the ceramsite concrete base material, continuing the microwave treatment for 40min, demoulding, putting the mixture into a 0.8MPa reaction kettle, heating to 670 ℃ at the speed of 10 ℃/min, carrying out heat preservation for 4h, heating to 1300 ℃, and carrying out heat preservation for 7h to prepare the ceramsite concrete material.
Comparative example 4
Comparative example 4 differs from example 2 only in step (2), step (2) being modified: mixing composite ceramsite, light sand, quicklime, cement and 70 ℃ deionized water according to a mass ratio of 1: 0.4: 0.15: 0.8: 1.2, mixing, shearing at 4750r/min for 5h, pouring into a mould at 50 ℃ for fixing for 5h, and drying at 85 ℃ for 24h to obtain the ceramsite concrete base material. The rest of the preparation steps are the same as example 2.
Comparative example 5
Comparative example 5 differs from example 2 only in step (3), step (3) being modified: under the conditions of room temperature and argon protection, placing a ceramsite concrete base material into a 4MPa closed container, dropwise adding a 30% sodium hydroxide solution at a rate of 60 drops/min, adjusting the pH value to 9, standing for 2h, and then mixing the materials in a mass ratio of 1: 10, adding zinc oxide and pyridine, wherein the mass of the zinc oxide is 0.013 times of that of the ceramsite concrete base material, carrying out ultrasonic treatment for 15min at 35kHz, carrying out microwave treatment for 20min under the microwave conditions of 2450MHz and 800W, adding dimethyl sulfate which is 0.02 times of that of the ceramsite concrete base material, continuing the microwave treatment for 40min, demoulding, putting the mixture into a 0.8MPa reaction kettle, heating to 670 ℃ at the speed of 10 ℃/min, carrying out heat preservation for 4h, heating to 1300 ℃, and carrying out heat preservation for 7h to prepare the ceramsite concrete material. The rest of the preparation steps are the same as example 2.
Comparative example 6
Comparative example 6 differs from example 2 only in step (3), step (3) being modified: at room temperature and under the protection of argon, mixing chlorinated polypropylene with molecular weight of 2000 and benzoic acid according to a mass ratio of 1: 4, mixing, stirring for 15min at 500r/min, adding aluminum trichloride of which the mass is 0.02 time that of chlorinated polypropylene, cooling to 2 ℃ at 3 ℃/min, stirring for 8h at 700r/min, and preparing to obtain polyacrylic benzoic acid; under the conditions of room temperature and argon protection, the method comprises the following steps of mixing propenylbenzoic acid and formamide according to a mass ratio of 1: 0.7, stirring at 500r/min for 25min, then adding nano titanium dioxide with the mass of 0.07 time of that of the acrylic benzoic acid, heating to 90 ℃ at 9.5 ℃/min, and continuously stirring for 3h to prepare the polyacrylic benzoic acid formamide; placing a ceramsite concrete base material into a 4MPa closed container under the conditions of room temperature and argon protection, pouring polyacrylic benzoic acid formamide with the mass of 0.5 time of that of the ceramsite concrete base material, dropwise adding 30% by mass of sodium hydroxide solution at a rate of 60 drops/min, adjusting the pH value to 9, standing for 2 hours, and then, mixing the raw materials according to a mass ratio of 1: 10, adding zinc oxide and pyridine, wherein the mass of the zinc oxide is 0.013 times of that of the ceramsite concrete base material, carrying out ultrasonic treatment for 15min at 35kHz, carrying out microwave treatment for 20min under the microwave conditions of 2450MHz and 800W, adding dimethyl sulfate which is 0.02 times of that of the ceramsite concrete base material, continuing the microwave treatment for 40min, and demoulding to prepare the ceramsite concrete material. The rest of the preparation steps are the same as example 2.
Examples of effects
The following table 1 shows the analysis results of the thermal insulation performance, the flame retardant performance, the anti-cracking performance and the toughness of the thermal insulation ceramsite concrete material prepared by the embodiments 1 to 3 and the comparative examples 1 to 6 of the invention.
TABLE 1
Figure BDA0003674565090000101
The table 1 shows that the thermal insulation ceramsite concrete materials prepared in the embodiments 1, 2 and 3 have strong thermal insulation performance, flame retardant performance, anti-cracking performance and toughness; the experimental data comparison of the examples 1, 2 and 3 and the comparative example 1 shows that the composite ceramsite prepared by using the tetraphenyl silicate can form carbon nanowires and silica aerogel in the composite ceramsite, and the prepared thermal insulation ceramsite concrete material has strong thermal insulation property and toughness; from the experimental data of the examples 1, 2 and 3 and the comparative example 2, it can be found that the composite ceramsite prepared by using the trimethyl aluminate can form carbon nanowires in the composite ceramsite, aluminum nitride grains can be formed when the thermal insulation ceramsite concrete material is prepared subsequently, and the prepared thermal insulation ceramsite concrete material has stronger toughness and anti-cracking performance; from the experimental data of the examples 1, 2 and 3 and the comparative example 3, it can be found that the thermal insulation ceramsite concrete material prepared by using the composite ceramsite prepared by using the tetraphenyl silicate and the trimethyl aluminate can form carbon nanowires and aluminum nitride grains, and the prepared thermal insulation ceramsite concrete material has stronger toughness and anti-cracking performance; from the experimental data of the examples 1, 2 and 3 and the comparative example 4, it can be found that the heat-insulating ceramsite concrete material prepared by using phosphorus pentachloride can form a polypropylene network and aluminum nitride crystal grains which take cyclophosphazene as a center, and the prepared heat-insulating ceramsite concrete material has stronger flame retardant property and crack resistance; from the experimental data of the examples 1, 2 and 3 and the comparative example 5, it can be found that when the thermal insulation ceramsite concrete material is prepared by using the polypropylene benzamide, a polypropylene network and aluminum nitride crystal grains which take the cyclophosphazene as the center can be formed, and the prepared thermal insulation ceramsite concrete material has stronger flame retardant property and crack resistance; from the experimental data of the examples 1, 2 and 3 and the comparative example 6, it can be found that the aluminum nitride crystal grains can be formed by preparing the thermal insulation ceramsite concrete material by secondary calcination, and the prepared thermal insulation ceramsite concrete material has stronger anti-cracking performance.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Claims (10)

1. The heat-insulation ceramsite concrete material is characterized in that the heat-insulation ceramsite concrete material is prepared by carrying out secondary calcination on a ceramsite concrete base material by utilizing polypropylene benzoic acid formamide.
2. The ceramsite concrete material according to claim 1, wherein the ceramsite concrete base material is prepared by mixing phosphorus pentachloride, composite ceramsite, light sand, quicklime, cement and water.
3. The thermal insulation ceramsite concrete material according to claim 2, wherein the composite ceramsite is prepared by mixing tetraphenyl silicate and trimethyl aluminate and then calcining the mixture.
4. The preparation method of the heat-insulation ceramsite concrete material is characterized by comprising the following preparation steps of:
(1) mixing composite ceramsite, light sand, quicklime, cement and 60-80 ℃ deionized water according to a mass ratio of 1: 0.3: 0.14: 0.7: 1.1-1: 0.5: 0.16: 0.9: 1.3, mixing, shearing for 4-6 h at 4500-5000 r/min, adding phosphorus pentachloride with the mass 0.6-0.8 time of that of the composite ceramsite, shearing for 4-6 h, pouring into a mold at 48-52 ℃ for fixation for 4-6 h, and drying at 80-90 ℃ for 23-25 h to obtain a ceramsite concrete base material;
(2) placing a ceramsite concrete base material into a closed container with the pressure of 3-5 MPa at room temperature under the protection of argon, pouring polyacrylic benzoic acid formamide with the mass of 0.4-0.6 time of that of the ceramsite concrete base material, dropwise adding 30% by mass of sodium hydroxide solution at the rate of 60 drops/min, adjusting the pH value to 9, standing for 1-3 h, and then, mixing the raw materials in a mass ratio of 1: 8-1: 12, adding zinc oxide and pyridine, wherein the mass of the zinc oxide is 0.01-0.016 times of that of the ceramsite concrete base material, performing ultrasonic treatment for 10-20 min at 30-40 kHz, performing microwave treatment for 15-25 min under the microwave conditions of 2400-2500 MHz and 700-900W, adding dimethyl sulfate which is 0.01-0.03 times of that of the ceramsite concrete base material, continuing performing microwave treatment for 30-50 min, demolding, putting the mixture into a reaction kettle with the pressure of 0.7-0.9 MPa, heating to 660-680 ℃ at 9-11 ℃/min, keeping the temperature for 2-6 h, heating to 1200-1400 ℃, and keeping the temperature for 4-10 h to prepare the ceramsite concrete material.
5. The method for preparing the thermal insulation ceramsite concrete material according to claim 4, wherein the method for preparing the composite ceramsite in the step (1) comprises the following steps: the composite sol is put into a refrigerator with the temperature of-4 to-2 ℃ for freezing for 47-49 h, dried for 47-49 h at the temperature of-10 to 20Pa and-50 to-40 ℃, washed for 2-4 times by absolute ethyl alcohol, put into a drying oven with the temperature of 10-20 Pa and 19-21 ℃ for drying for 1-3 h, then soaked in a nickel nitrate solution with the mass fraction of 10% and the mass ratio of 0.2-0.3 times of that of the composite sol for 10-20 h, taken out and put into a reaction kettle with the pressure of 0.7-0.9 MPa, heated to 690-710 ℃ at the speed of 9-11 ℃/min, insulated for 1-3 h, heated to 1300-1500 ℃ for heat preservation for 1-3 h, naturally cooled to the normal temperature, washed for 3-5 times by absolute ethyl alcohol, put into a drying oven with the temperature of 30-40 ℃ for drying for 1-3 h, and the composite ceramsite is prepared.
6. The preparation method of the thermal insulation ceramsite concrete material according to claim 5, wherein the preparation method of the composite sol comprises the following steps: under the conditions of 80-90 ℃ and argon protection, trimethyl aluminate and deionized water are mixed according to the mass ratio of 1: 7-1: 9, stirring for 1-3 hours at 400-600 r/min, dripping a nitric acid solution with the mass fraction of 11-13% and the mass of 0.2-0.3 times of that of trimethyl aluminate at 40-60 drops/min, continuously stirring for 1-3 hours, adding silver with the mass of 0.01-0.03 times of that of trimethyl aluminate, heating to 500-560 ℃ at 9-11 ℃/min, keeping the temperature for 8-10 hours, cooling to 24-26 ℃ at 9-11 ℃/min, adding tetraphenyl silicate with the mass of 2-4 times of that of trimethyl aluminate, continuously dripping ethanol with the mass of 8-16 times of that of trimethyl aluminate, continuously stirring for 2-4 hours at 60-80 ℃, adding ammonium hydroxide with the mass of 0.08-0.16 times of that of trimethyl aluminate, continuously stirring for 10-20 minutes, heating to 65-85 ℃ at 2-4 ℃/min, continuously stirring for 10-20 minutes, continuously heating to 95-105 ℃, stirring for 60-80 minutes at 600-800 r/min, and preparing the composite sol.
7. The method for preparing the thermal insulation ceramsite concrete material according to claim 4, wherein the light sand in the step (1) has a fineness modulus of 1.6 and an apparent density of 2870kg/m 3 The natural river sand.
8. The preparation method of the thermal insulation ceramsite concrete material according to claim 4, wherein the preparation method of the polyacrylic benzoic acid amide in the step (2) is as follows: under the conditions of room temperature and argon protection, the method comprises the following steps of mixing propenylbenzoic acid and formamide according to a mass ratio of 1: 0.6-1: 0.8, stirring for 20-30 min at 400-600 r/min, then adding nano titanium dioxide which is 0.06-0.08 times of the mass of the acrylic benzoic acid, heating to 80-100 ℃ at 9-10 ℃/min, and continuously stirring for 2-4 h to prepare the polyacrylic benzoic acid formamide.
9. The method for preparing the heat-insulating ceramsite concrete material according to claim 8, wherein the method for preparing the polyacrylic benzoic acid comprises the following steps: at room temperature and under the protection of argon, mixing chlorinated polypropylene and benzoic acid according to a mass ratio of 1: 3-1: 5, mixing, stirring for 10-20 min at 400-600 r/min, adding aluminum trichloride of which the mass is 0.01-0.03 time that of chlorinated polypropylene, cooling to 0-4 ℃ at 2-4 ℃/min, stirring for 7-9 h at 600-800 r/min, and thus obtaining the polyacrylic benzoic acid.
10. The method for preparing the heat-insulating ceramsite concrete material according to claim 9, wherein the molecular weight of the chlorinated polypropylene is 1000-3000.
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