CN115772014B - Preparation method of heat-insulating ceramsite concrete material - Google Patents

Preparation method of heat-insulating ceramsite concrete material Download PDF

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CN115772014B
CN115772014B CN202211344496.5A CN202211344496A CN115772014B CN 115772014 B CN115772014 B CN 115772014B CN 202211344496 A CN202211344496 A CN 202211344496A CN 115772014 B CN115772014 B CN 115772014B
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ceramsite
mass
composite
temperature
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CN115772014A (en
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张皓
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Guangzhou Suifan Concrete Co ltd
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Guangzhou Suifan Concrete Co ltd
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Abstract

The invention discloses a preparation method of a heat-insulating ceramsite concrete material, and relates to the technical field of concrete. Mixing tetraphenyl silicate and trimethyl aluminate, and calcining for the first time to form silica aerogel, alumina and carbon nano wires, so as to prepare 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 using polypropylene benzoic acid formamide to form a polypropylene network with cyclophosphazene as a center, and performing partial polypropylene network calcination to form a compact carbon layer and nitrogen, wherein aluminum formed by reducing aluminum oxide by the compact carbon layer reacts with the nitrogen to form aluminum nitride grains, so as to prepare the heat-insulating ceramsite concrete material; the heat-insulating ceramsite concrete material prepared by the invention has good heat-insulating property, flame retardant property, anti-cracking property and toughness.

Description

Preparation method of heat-insulating ceramsite concrete material
Technical Field
The invention relates to the technical field of concrete, in particular to a preparation method of a heat-insulating ceramsite concrete material.
Background
The concrete is a composite material which is formed by configuring gel materials, aggregate and water according to proper proportion and hardening for a certain time, and is a common name of artificial civil construction materials with the largest use 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, highways, military projects, nuclear power plants and other structures.
Along with the development of society and the rapid promotion of living standard, the demand of people on buildings is increased, and the concrete is gradually developed towards the direction of light heat preservation, wherein, the haydite concrete is made of haydite instead of stone as the aggregate of the concrete, and the haydite concrete is light and heat preservation because of loose and porous structure, thus, the haydite concrete is also a lightweight aggregate concrete, and therefore, the haydite concrete is also outstanding from a plurality of 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, has insufficient fire resistance, has more potential safety hazards and greatly influences the application of the ceramsite concrete. The present invention addresses this situation and solves these problems by preparing a thermal insulating ceramsite concrete material.
Disclosure of Invention
The invention aims to provide a heat-insulating ceramsite concrete material and a preparation method thereof, which are used for solving 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 performing secondary calcination on a ceramsite concrete base material by using polypropylene-based benzoic acid formamide.
Further, 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-preservation ceramsite concrete material comprises the following preparation steps:
(1) The method comprises the following steps of (1) mixing composite ceramsite, light sand, quicklime, cement and deionized water at 60-80 ℃ 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 hours at 4500-5000 r/min, then adding phosphorus pentachloride with the mass of 0.6-0.8 times of that of the composite ceramsite, shearing for 4-6 hours, pouring into a mould at 48-52 ℃ for fixing for 4-6 hours, and drying at 80-90 ℃ for 23-25 hours to obtain ceramsite concrete base material;
(2) Under the conditions of room temperature and argon protection, placing a ceramsite concrete base material into a closed container with the pressure of 3-5 MPa, pouring polypropylene-based benzoic acid formamide with the mass of 0.4-0.6 times of that of the ceramsite concrete base material, dripping sodium hydroxide solution with the mass fraction of 30% at 60 drops/min, regulating the pH value to 9, standing for 1-3 h, and then, according to the 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 that of the ceramsite concrete base material, carrying out ultrasonic treatment for 10-20 min at 30-40 kHz, carrying out microwave treatment for 15-25 min under the microwave conditions of 2400-2500 MHz and 700-900W, adding dimethyl sulfate with the mass of 0.01-0.03 times that of the ceramsite concrete base material, continuing to carry out microwave treatment for 30-50 min, demolding, putting into a reaction kettle with the pressure of 0.7-0.9 MPa, heating to 660-680 ℃ at 9-11 ℃/min, carrying out heat preservation for 2-6 h, heating to 1200-1400 ℃, and carrying out heat preservation for 4-10 h, thus obtaining the ceramsite concrete material.
Further, the preparation method of the composite ceramsite in the step (1) comprises the following steps: putting the composite sol into a refrigerator with the temperature ranging from minus 4 ℃ to minus 2 ℃ to be cooled for 47-49 h, drying at the temperature ranging from 10Pa to 20Pa to minus 50 ℃ to minus 40 ℃ for 47-49 h, washing with absolute ethyl alcohol for 2-4 times, putting into a baking oven with the temperature ranging from 10Pa to 20Pa and 19-21 ℃ to be baked for 1-20 h, soaking into a nickel nitrate solution with the mass fraction ranging from 10% and 0.2-0.3 times of the mass of the composite sol for 10-20 h, taking out, putting into a reaction kettle with the pressure ranging from 0.7MPa to 0.9MPa, heating to 690-710 ℃ at the speed ranging from 9 ℃/min, heating to 1300-1500 ℃ after the temperature is kept for 1-3 h, naturally cooling to normal temperature, washing with absolute ethyl alcohol for 3-5 times, and putting into a baking oven with the temperature ranging from 30-40 ℃ to be baked for 1-3 h, thus obtaining the composite ceramsite.
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, mixing, stirring for 1-3 hours at 400-600 r/min, dropwise adding nitric acid solution with the mass fraction of 11-13% and the mass fraction of trimethyl aluminate of 0.2-0.3 times that of the trimethyl aluminate of 40-60 r/min, continuously stirring for 1-3 hours, adding silver with the mass of 0.01-0.03 times that of the trimethyl aluminate, heating to 500-560 ℃ at 9-11 ℃/min, preserving heat for 8-10 hours, cooling to 24-26 ℃ at 9-11 ℃/min, adding tetraphenyl silicate with the mass of 2-4 times that of the trimethyl aluminate, continuously dropwise adding ethanol with the mass of 8-16 times that of the trimethyl aluminate, continuously stirring for 2-4 hours at 60-80 ℃, adding ammonium hydroxide with the mass of 0.08-0.16 times that of the trimethyl aluminate, continuously stirring for 10-20 min, heating to 65-85 ℃ at 2-4 ℃/min, continuously stirring for 10-20 min, continuously heating to 95-105 ℃, and stirring for 60-80 min at 600-800 r/min to prepare the composite sol.
Further, the light sand in the step (1) has a fineness modulus of 1.6 and an apparent density of 2870kg/m 3 Is a natural river sand.
Further, the preparation method of the polypropylene-based benzoic acid formamide in the step (2) comprises the following steps: under the conditions of room temperature and argon protection, the mass ratio of the propenyl benzoic acid to the formamide is 1: 0.6-1: mixing 0.8, stirring for 20-30 min at 400-600 r/min, then adding nano titanium dioxide with the mass of 0.06-0.08 times that of propenyl benzoic acid, heating to 80-100 ℃ at 9-10 ℃/min, and continuously stirring for 2-4 h to obtain the polypropylene benzoic acid formamide.
Further, the preparation method of the polypropylene-based benzoic acid comprises the following steps: under the conditions of high temperature and argon protection, chlorinated polypropylene and benzoic acid are mixed according to the mass ratio of 1: 3-1: 5, mixing, stirring for 10-20 min at 400-600 r/min, adding aluminum trichloride with the mass of 0.01-0.03 times of that of the chlorinated polypropylene, cooling to 0-4 ℃ at 2-4 ℃/min, and stirring for 7-9 h at 600-800 r/min to obtain the polypropylene-based benzoic acid.
Further, 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-insulating ceramsite concrete material is prepared, tetraphenyl silicate and trimethyl aluminate are mixed and calcined for the first time, so that composite ceramsite is prepared; mixing phosphorus pentachloride, composite ceramsite, light sand, cement, quicklime and water to prepare a ceramsite concrete base material; finally, the polypropylene benzoic acid formamide is utilized to carry out secondary calcination on the ceramsite concrete base material, and the heat-preservation ceramsite concrete material is prepared.
Firstly, tetraphenyl silicate and trimethyl aluminate are hydrolyzed, phenol and methanol are removed, and then the reaction crosslinking is carried out, so that silicon dioxide aerogel and aluminum oxide are formed, and the heat preservation performance of the composite ceramsite is enhanced; methanol is oxidized to form formaldehyde, the formaldehyde reacts with phenol to crosslink, a phenolic network is formed, 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 pinned together, so that the toughness of the composite ceramsite is enhanced.
Secondly, part of phosphorus pentachloride is hydrolyzed to form phosphoric acid and hydrogen chloride, phosphoric acid activates ceramsite concrete base materials, a large number of free radicals such as hydroxyl are formed in the ceramsite concrete base materials, polyacrylamide is hydrolyzed to form formamide and polyacrylamide, the formamide is decomposed and reacts with hydrogen chloride to form ammonium chloride, and the ammonium chloride reacts with part of phosphorus pentachloride to form hexachlorocyclophosphazene, so that the flame retardant property of the heat-insulating ceramsite concrete material is enhanced; carboxyl on the polypropylene-based benzoic acid reacts with hydroxyl in the ceramsite concrete base material to crosslink, benzene ring on the hexachlorocyclophosphazene and the polypropylene-based benzoic acid reacts and crosslinks to form a polypropylene network taking the cyclophosphazene as a center, when the polypropylene network is calcined, part of the cyclophosphazene is taken as an acid source and an air source, and the polypropylene-based 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, the carbon layer reduces alumina in the composite ceramsite into aluminum, part of melted aluminum flows out of the composite ceramsite to react with the nitrogen to form aluminum nitride crystal grains, and the composite ceramsite and the cement base material are firmly embedded together, so that the cracking resistance of the thermal insulation ceramsite concrete material is enhanced.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below 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.
In order to more clearly illustrate the method provided by the invention, the following examples are used for describing the detailed description, and the method for testing each index of the heat-insulating ceramsite concrete material prepared in the following examples is as follows:
thermal insulation performance: the heat-insulating ceramsite concrete materials prepared by the examples and the comparative examples with the same mass are used for measuring the heat conductivity coefficient according to the GB/T10295 standard method to measure the heat-insulating property.
Flame retardant properties: the heat-insulating ceramsite concrete materials prepared by the examples and the comparative examples with the same quality are tested for flame retardance according to the oxygen index of GB/T29051 standard method.
Crack resistance: the thermal insulation ceramsite concrete materials prepared by the examples and the comparative examples with the same length and width are used for measuring the splitting tensile strength according to the GB/T50081 standard method to measure the anti-cracking performance.
Toughness: the ultrafine grain titanium-based high-plasticity ceramic materials prepared by the examples and the comparative examples with the same length and width are used for testing the fracture toughness according to ASTMC 1421.
Example 1
The preparation method of the heat-preservation 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, namely, dropwise adding nitric acid solution with the mass fraction of 11% and the mass fraction of 0.2 times of trimethyl aluminate at 400r/min for 1h, continuously stirring for 1h, adding silver with the mass fraction of 0.01 times of trimethyl aluminate, heating to 500 ℃ at 9 ℃/min for 8h, cooling to 24 ℃ at 9 ℃/min, adding tetraphenyl silicate with the mass fraction of 2 times of trimethyl aluminate, continuously dropwise adding ethanol with the mass fraction of 8 times of trimethyl aluminate, continuously stirring for 2h at 60 ℃, adding ammonium hydroxide with the mass fraction of 0.08 times 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 obtain composite sol; freezing the composite sol in a refrigerator at the temperature of minus 4 ℃ for 47 hours, drying for 47 hours at the temperature of 10Pa and minus 50 ℃, washing for 2 times by using absolute ethyl alcohol, putting into a baking oven at the temperature of 10Pa and 19 ℃ for baking for 1 hour, soaking in nickel nitrate solution with the mass fraction of 10% which is 0.2 times of the mass of the composite sol for 10 hours, taking out, putting into a reaction kettle at the temperature of 0.7MPa, heating to 690 ℃ at the speed of 9 ℃/min, keeping the temperature for 1 hour, heating to 1300 ℃ and keeping the temperature for 1 hour, naturally cooling to normal temperature, washing for 3 times by using absolute ethyl alcohol, and putting into a baking oven at the temperature of 30 ℃ for baking for 1 hour to prepare the composite ceramsite;
(2) The method comprises the following steps of (1) 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 4 hours at 4500r/min, then adding phosphorus pentachloride with the mass of 0.6 times of that of the composite ceramsite, shearing for 4 hours, pouring into a mould at 48 ℃ for fixing for 4 hours, and drying at 80 ℃ for 23 hours to obtain ceramsite concrete base material;
(3) Under the protection of argon at the temperature, chlorinated polypropylene with the molecular weight of 1000 and benzoic acid are mixed according to the mass ratio of 1:3 mixing, stirring for 10min at 400r/min, adding aluminum trichloride with the mass of 0.01 times that of the chlorinated polypropylene, cooling to 0 ℃ at 2 ℃/min, and stirring for 7h at 600r/min to prepare the polypropylene-based benzoic acid; under the conditions of room temperature and argon protection, the mass ratio of the propenyl benzoic acid to the formamide is 1:0.6, mixing, stirring for 20min at 400r/min, then adding nano titanium dioxide with the mass of 0.06 times that of the propenyl benzoic acid, heating to 80 ℃ at 9 ℃/min, and continuously stirring for 2h to prepare the polypropylene benzoic acid formamide; under the conditions of room temperature and argon protection, placing a ceramsite concrete base material into a closed container with the pressure of 3MPa, pouring polypropylene-based benzoic acid formamide with the mass of 0.4 times of that of the ceramsite concrete base material, dropwise adding a sodium hydroxide solution with the mass fraction of 30% at 60 drops/min, regulating the pH value to 9, standing for 1h, and then, according to the mass ratio of 1:8, adding zinc oxide and pyridine, wherein the mass of the zinc oxide is 0.01 times of that of the ceramsite concrete base material, carrying out ultrasonic treatment for 10min at 30kHz, carrying out microwave treatment for 15min under 2400MHz and 700W microwave conditions, adding dimethyl sulfate with the mass of 0.01 times of that of the ceramsite concrete base material, continuing microwave treatment for 30min, demolding, putting into a reaction kettle with the pressure of 0.7MPa, heating to 660 ℃ at 9 ℃/min, carrying out heat preservation for 2h, heating to 1200 ℃, and carrying out heat preservation for 4h, thus obtaining the ceramsite concrete material.
Example 2
The preparation method of the heat-preservation 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, namely, dropwise adding nitric acid solution with the mass fraction of 12% and the mass fraction of 0.25 times of trimethyl aluminate at 500r/min for 2h, continuously stirring for 2h, adding silver with the mass fraction of 0.02 times of trimethyl aluminate, heating to 530 ℃ at 10 ℃/min for 9h, cooling to 25 ℃ at 10 ℃/min, adding tetraphenyl silicate with the mass fraction of 3 times of trimethyl aluminate, continuously dropwise adding ethanol with the mass fraction of 12 times of trimethyl aluminate, continuously stirring for 3h at 70 ℃, adding ammonium hydroxide with the mass fraction of 0.12 times of trimethyl aluminate, continuously stirring for 15min, heating to 75 ℃ at 3 ℃/min, continuously stirring for 15min, continuously heating to 100 ℃ and stirring for 70min at 700r/min to prepare the composite sol; freezing the composite sol in a refrigerator at the temperature of minus 3 ℃ for 48 hours, drying the composite sol at the temperature of 15Pa and minus 45 ℃ for 48 hours, washing the composite sol with absolute ethyl alcohol for 3 times, putting the composite sol in a baking oven at the temperature of 15Pa and 20 ℃ for 2 hours, immersing the composite sol in nickel nitrate solution with the mass fraction of 10% which is 0.25 times of the mass of the composite sol for 15 hours, taking out the composite sol, putting the composite sol into a reaction kettle at the pressure of 0.8MPa, heating the composite sol to 700 ℃ at the temperature of 10 ℃/min, keeping the temperature for 2 hours, heating the composite sol to 1400 ℃, keeping the temperature for 2 hours, naturally cooling the composite sol to normal temperature, washing the composite sol with absolute ethyl alcohol for 4 times, and putting the composite ceramsite in a baking oven at the temperature of 35 ℃ for 2 hours to prepare the composite ceramsite;
(2) The method comprises the following steps of (1) 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 5 hours at 4750r/min, then adding phosphorus pentachloride with the mass 0.7 times of that of the composite ceramsite, shearing for 5 hours, pouring into a mould at 50 ℃ for fixing for 5 hours, and drying at 85 ℃ for 24 hours to obtain a ceramsite concrete base material;
(3) Under the protection of argon at the temperature, chlorinated polypropylene with the molecular weight of 2000 and benzoic acid are mixed according to the mass ratio of 1:4, mixing, stirring for 15min at 500r/min, adding aluminum trichloride with the mass which is 0.02 times that of the chlorinated polypropylene, cooling to 2 ℃ at 3 ℃/min, and stirring for 8h at 700r/min to prepare the polypropylene-based benzoic acid; under the conditions of room temperature and argon protection, the mass ratio of the propenyl benzoic acid to the formamide is 1:0.7, mixing, stirring for 25min at 500r/min, then adding nano titanium dioxide with the mass 0.07 times of that of the propenyl benzoic acid, heating to 90 ℃ at 9.5 ℃/min, and continuously stirring for 3h to prepare the polypropylene benzoic acid formamide; under the conditions of room temperature and argon protection, placing a ceramsite concrete base material into a 4MPa closed container, pouring polypropylene-based benzoic acid formamide with the mass of 0.5 times of that of the ceramsite concrete base material, dropwise adding a sodium hydroxide solution with the mass fraction of 30% at 60 drops/min, regulating the pH value to 9, standing for 2 hours, and then, according to the 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 2450MHz and 800W microwave conditions, adding dimethyl sulfate with the mass of 0.02 times of that of the ceramsite concrete base material, continuing microwave treatment for 40min, demolding, putting into a reaction kettle with the pressure of 0.8MPa, heating to 670 ℃ at 10 ℃/min, carrying out heat preservation for 4h, heating to 1300 ℃, and carrying out heat preservation for 7h, thus obtaining the ceramsite concrete material.
Example 3
The preparation method of the heat-preservation 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, namely, stirring for 3 hours at 600r/min, dropwise adding a nitric acid solution with the mass fraction of 13% and with the mass fraction of 0.3 times that of trimethyl aluminate at 60 r/min, continuously stirring for 3 hours, adding silver with the mass fraction of 0.03 times 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 fraction of 4 times that of trimethyl aluminate, continuously dropwise adding ethanol with the mass fraction of 16 times that of trimethyl aluminate, continuously stirring for 4 hours at 80 ℃, adding ammonium hydroxide with the mass fraction of 0.16 times that of trimethyl aluminate, continuously stirring for 20 minutes, heating to 85 ℃ at 4 ℃/min, continuously stirring for 20 minutes, continuously heating to 105 ℃, and stirring for 80 minutes at 800r/min to obtain composite sol; freezing the composite sol in a refrigerator at the temperature of minus 2 ℃ for 49 hours, drying the composite sol at the temperature of 20Pa and minus 40 ℃ for 49 hours, washing the composite sol with absolute ethyl alcohol for 4 times, putting the composite sol in an oven at the temperature of 20Pa and 21 ℃ for 3 hours, immersing the composite sol in nickel nitrate solution with the mass fraction of 10% which is 0.3 times of the mass of the composite sol for 20 hours, taking out the composite sol, putting the composite sol into a reaction kettle at the pressure of 0.9MPa, heating the composite sol to 710 ℃ at the temperature of 11 ℃/min, keeping the temperature for 3 hours, heating the composite sol to 1500 ℃, keeping the temperature for 3 hours, naturally cooling the composite sol to normal temperature, washing the composite sol with absolute ethyl alcohol for 5 times, and putting the composite sol into an oven at the temperature of 40 ℃ for 3 hours to prepare composite ceramsite;
(2) The method comprises the following steps of (1) 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 6 hours at 5000r/min, then adding phosphorus pentachloride with the mass 0.8 times of that of the composite ceramsite, shearing for 6 hours, pouring into a mould at 52 ℃ for fixing for 6 hours, and drying for 25 hours at 90 ℃ to obtain a ceramsite concrete base material;
(3) Under the protection of argon at the temperature, chlorinated polypropylene with the molecular weight of 3000 and benzoic acid are mixed according to the mass ratio of 1:5, mixing, stirring for 20min at 600r/min, adding aluminum trichloride with the mass of 0.03 times that of the chlorinated polypropylene, cooling to 4 ℃ at 4 ℃ per min, and stirring for 9h at 800r/min to prepare the polypropylene-based benzoic acid; under the conditions of room temperature and argon protection, the mass ratio of the propenyl benzoic acid to the formamide is 1: mixing 0.8, stirring at 600r/min for 30min, then adding nano titanium dioxide with the mass of 0.08 times that of the propenyl benzoic acid, heating to 100 ℃ at 10 ℃/min, and continuously stirring for 4h to prepare the polypropylene benzoic acid formamide; under the conditions of room temperature and argon protection, placing a ceramsite concrete base material into a sealed container with the pressure of 5MPa, pouring polypropylene-based benzoic acid formamide with the mass of 0.6 times of that of the ceramsite concrete base material, dropwise adding a sodium hydroxide solution with the mass fraction of 30% at 60 drops/min, regulating the pH value to 9, standing for 3 hours, and then, 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 condition of 2500MHz and 900W, adding dimethyl sulfate with the mass of 0.03 times of that of the ceramsite concrete base material, continuing the microwave treatment for 50min, demoulding, putting into a reaction kettle with the pressure of 0.9MPa, heating to 680 ℃ at 11 ℃/min, carrying out heat preservation for 6h, heating to 1400 ℃, and carrying out heat preservation for 10h, thus obtaining the ceramsite concrete material.
Comparative example 1
Comparative example 1 differs from example 2 only in the difference of step (1), the step (1) was modified as: under the conditions of 85 ℃ and argon protection, trimethyl aluminate and deionized water are mixed according to the mass ratio of 1:8, mixing, namely, dropwise adding nitric acid solution with the mass fraction of 12% and the mass fraction of 0.25 times that of trimethyl aluminate at 500r/min for 2h, continuously stirring for 2h, adding silver with the mass fraction of 0.02 times that of trimethyl aluminate, heating to 530 ℃ at 10 ℃/min, preserving heat for 9h, cooling to 25 ℃ at 10 ℃/min, continuously dropwise adding ethanol with the mass fraction of 12 times that of trimethyl aluminate, continuously stirring for 3h at 70 ℃, adding ammonium hydroxide with the mass fraction of 0.12 times that of trimethyl aluminate, continuously stirring for 15min, heating to 75 ℃ at 3 ℃/min, continuously stirring for 15min, continuously heating to 100 ℃, and stirring for 70min at 700r/min to prepare the composite sol; freezing the composite sol in a refrigerator at the temperature of minus 3 ℃ for 48 hours, drying the composite sol at the temperature of 15Pa and minus 45 ℃ for 48 hours, washing the composite sol with absolute ethyl alcohol for 3 times, putting the composite sol in a baking oven at the temperature of 15Pa and 20 ℃ for 2 hours, immersing the composite sol in nickel nitrate solution with the mass fraction of 10% which is 0.25 times of the mass of the composite sol for 15 hours, taking out the composite sol, putting the composite sol into a reaction kettle at the pressure of 0.8MPa, heating the composite sol to 700 ℃ at the temperature of 10 ℃/min, keeping the temperature for 2 hours, heating the composite sol to 1400 ℃, keeping the temperature for 2 hours, naturally cooling the composite sol to normal temperature, washing the composite sol with absolute ethyl alcohol for 4 times, and putting the composite ceramsite in a baking oven at the temperature of 35 ℃ for 2 hours. The remaining preparation steps were the same as in example 2.
Comparative example 2
Comparative example 2 differs from example 2 only in the difference of step (1), the step (1) was modified as: at 25 ℃, tetraphenyl silicate and ethanol are mixed according to the mass ratio of 1:4, mixing, stirring for 25min at 500r/min, then dripping nitric acid solution with mass fraction of 12% which is 0.25 times of that of tetraphenyl silicate at 50 drops/min, continuously stirring for 3h at 85 ℃, and naturally cooling to room temperature to prepare composite sol; freezing the composite sol in a refrigerator at the temperature of minus 3 ℃ for 48 hours, drying the composite sol at the temperature of 15Pa and minus 45 ℃ for 48 hours, washing the composite sol with absolute ethyl alcohol for 3 times, putting the composite sol in a baking oven at the temperature of 15Pa and 20 ℃ for 2 hours, immersing the composite sol in nickel nitrate solution with the mass fraction of 10% which is 0.25 times of the mass of the composite sol for 15 hours, taking out the composite sol, putting the composite sol into a reaction kettle at the pressure of 0.8MPa, heating the composite sol to 700 ℃ at the temperature of 10 ℃/min, keeping the temperature for 2 hours, heating the composite sol to 1400 ℃, keeping the temperature for 2 hours, naturally cooling the composite sol to normal temperature, washing the composite sol with absolute ethyl alcohol for 4 times, and putting the composite ceramsite in a baking oven at the temperature of 35 ℃ for 2 hours. The remaining preparation steps were the same as in example 2.
Comparative example 3
The preparation method of the heat-preservation ceramsite concrete material comprises the following preparation steps:
(1) Shale ceramsite, light sand, quicklime, cement and 70 ℃ deionized water are mixed according to the mass ratio of 1:0.4:0.15:0.8:1.2, mixing, shearing for 5 hours at 4750r/min, then adding phosphorus pentachloride with the mass 0.7 times of that of shale ceramsite, shearing for 5 hours, pouring into a mould at 50 ℃ for fixing for 5 hours, and drying at 85 ℃ for 24 hours to obtain ceramsite concrete base material;
(2) Under the protection of argon at the temperature, chlorinated polypropylene with the molecular weight of 2000 and benzoic acid are mixed according to the mass ratio of 1:4, mixing, stirring for 15min at 500r/min, adding aluminum trichloride with the mass which is 0.02 times that of the chlorinated polypropylene, cooling to 2 ℃ at 3 ℃/min, and stirring for 8h at 700r/min to prepare the polypropylene-based benzoic acid; under the conditions of room temperature and argon protection, the mass ratio of the propenyl benzoic acid to the formamide is 1:0.7, mixing, stirring for 25min at 500r/min, then adding nano titanium dioxide with the mass 0.07 times of that of the propenyl benzoic acid, heating to 90 ℃ at 9.5 ℃/min, and continuously stirring for 3h to prepare the polypropylene benzoic acid formamide; under the conditions of room temperature and argon protection, placing a ceramsite concrete base material into a 4MPa closed container, pouring polypropylene-based benzoic acid formamide with the mass of 0.5 times of that of the ceramsite concrete base material, dropwise adding a sodium hydroxide solution with the mass fraction of 30% at 60 drops/min, regulating the pH value to 9, standing for 2 hours, and then, according to the 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 2450MHz and 800W microwave conditions, adding dimethyl sulfate with the mass of 0.02 times of that of the ceramsite concrete base material, continuing microwave treatment for 40min, demolding, putting into a reaction kettle with the pressure of 0.8MPa, heating to 670 ℃ at 10 ℃/min, carrying out heat preservation for 4h, heating to 1300 ℃, and carrying out heat preservation for 7h, thus obtaining the ceramsite concrete material.
Comparative example 4
Comparative example 4 differs from example 2 only in the difference of step (2), the modification of step (2) to: the method comprises the following steps of (1) 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, shearing for 5 hours at 4750r/min, pouring into a mould at 50 ℃ for fixing for 5 hours, and then baking for 24 hours at 85 ℃ to obtain the ceramsite concrete base material. The remaining preparation steps were the same as in example 2.
Comparative example 5
Comparative example 5 differs from example 2 only in the difference of step (3), the modification of step (3) to: under the conditions of room temperature and argon protection, placing the ceramsite concrete base material into a closed container with the pressure of 4MPa, dropwise adding a sodium hydroxide solution with the mass fraction of 30% at 60 drops/min, adjusting the pH value to 9, standing for 2 hours, and then, according to the 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 2450MHz and 800W microwave conditions, adding dimethyl sulfate with the mass of 0.02 times of that of the ceramsite concrete base material, continuing microwave treatment for 40min, demolding, putting into a reaction kettle with the pressure of 0.8MPa, heating to 670 ℃ at 10 ℃/min, carrying out heat preservation for 4h, heating to 1300 ℃, and carrying out heat preservation for 7h, thus obtaining the ceramsite concrete material. The remaining preparation steps were the same as in example 2.
Comparative example 6
Comparative example 6 differs from example 2 only in the difference of step (3), the modification of step (3) to: under the protection of argon at the temperature, chlorinated polypropylene with the molecular weight of 2000 and benzoic acid are mixed according to the mass ratio of 1:4, mixing, stirring for 15min at 500r/min, adding aluminum trichloride with the mass which is 0.02 times that of the chlorinated polypropylene, cooling to 2 ℃ at 3 ℃/min, and stirring for 8h at 700r/min to prepare the polypropylene-based benzoic acid; under the conditions of room temperature and argon protection, the mass ratio of the propenyl benzoic acid to the formamide is 1:0.7, mixing, stirring for 25min at 500r/min, then adding nano titanium dioxide with the mass 0.07 times of that of the propenyl benzoic acid, heating to 90 ℃ at 9.5 ℃/min, and continuously stirring for 3h to prepare the polypropylene benzoic acid formamide; under the conditions of room temperature and argon protection, placing a ceramsite concrete base material into a 4MPa closed container, pouring polypropylene-based benzoic acid formamide with the mass of 0.5 times of that of the ceramsite concrete base material, dropwise adding a sodium hydroxide solution with the mass fraction of 30% at 60 drops/min, regulating the pH value to 9, standing for 2 hours, and then, according to the 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 2450MHz and 800W microwave conditions, adding dimethyl sulfate with the mass of 0.02 times of that of the ceramsite concrete base material, continuing microwave treatment for 40min, and demoulding to obtain the ceramsite concrete material. The remaining preparation steps were the same as in example 2.
Effect example
The following table 1 shows the analysis results of the heat insulation performance, flame retardant performance, crack resistance and toughness of the heat insulation ceramsite concrete materials prepared by using the examples 1 to 3 and the comparative examples 1 to 6 of the present invention.
TABLE 1
Figure 193905DEST_PATH_IMAGE002
From table 1, it can be found that the heat-insulating ceramsite concrete materials prepared in examples 1, 2 and 3 have strong heat-insulating property, flame-retardant property, cracking resistance and toughness; from comparison of experimental data of examples 1, 2 and 3 and comparative example 1, it can be found that the carbon nano-wires and the silica aerogel can be formed in the composite ceramsite by using tetraphenyl silicate to prepare the composite ceramsite, and the prepared heat-insulating ceramsite concrete material has stronger heat insulation property and toughness; from the experimental data of examples 1, 2 and 3 and comparative example 2, it can be found that the use of trimethyl aluminate for preparing composite ceramsite can form carbon nanowires in the composite ceramsite, and aluminum nitride grains can be formed when the thermal-insulation ceramsite concrete material is prepared subsequently, so that the prepared thermal-insulation ceramsite concrete material has stronger toughness and crack resistance; from the experimental data of examples 1, 2 and 3 and comparative example 3, it can be found that the composite ceramsite prepared from tetraphenyl silicate and trimethyl aluminate is used for preparing the heat-insulating ceramsite concrete material, carbon nano wires and aluminum nitride grains can be formed, and the toughness and crack resistance are stronger; from the experimental data of examples 1, 2, 3 and 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 grains with cyclophosphazene as the center, and the prepared heat-insulating ceramsite concrete material has stronger flame retardant property and crack resistance; from the experimental data of examples 1, 2 and 3 and comparative example 5, it can be found that the heat-insulating ceramsite concrete material prepared by using the polypropylene-based benzamide can form a polypropylene network and aluminum nitride grains with cyclophosphazene as the center, and the prepared heat-insulating ceramsite concrete material has stronger flame retardant property and crack resistance; from the experimental data of examples 1, 2 and 3 and comparative example 6, it can be found that aluminum nitride grains can be formed by preparing the heat-insulating ceramsite concrete material by secondary calcination, and the prepared heat-insulating ceramsite concrete material has stronger cracking resistance.
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 characteristics 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 (1)

1. A preparation method of a heat-insulating ceramsite concrete material is characterized by comprising the following steps: the preparation method 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, namely, dropwise adding nitric acid solution with the mass fraction of 12% and the mass fraction of 0.25 times of trimethyl aluminate at 500r/min for 2h, continuously stirring for 2h, adding silver with the mass fraction of 0.02 times of trimethyl aluminate, heating to 530 ℃ at 10 ℃/min for 9h, cooling to 25 ℃ at 10 ℃/min, adding tetraphenyl silicate with the mass fraction of 3 times of trimethyl aluminate, continuously dropwise adding ethanol with the mass fraction of 12 times of trimethyl aluminate, continuously stirring for 3h at 70 ℃, adding ammonium hydroxide with the mass fraction of 0.12 times of trimethyl aluminate, continuously stirring for 15min, heating to 75 ℃ at 3 ℃/min, continuously stirring for 15min, continuously heating to 100 ℃ and stirring for 70min at 700r/min to prepare the composite sol; freezing the composite sol in a refrigerator at the temperature of minus 3 ℃ for 48 hours, drying the composite sol at the temperature of 15Pa and minus 45 ℃ for 48 hours, washing the composite sol with absolute ethyl alcohol for 3 times, putting the composite sol in a baking oven at the temperature of 15Pa and 20 ℃ for 2 hours, immersing the composite sol in nickel nitrate solution with the mass fraction of 10% which is 0.25 times of the mass of the composite sol for 15 hours, taking out the composite sol, putting the composite sol into a reaction kettle at the pressure of 0.8MPa, heating the composite sol to 700 ℃ at the temperature of 10 ℃/min, keeping the temperature for 2 hours, heating the composite sol to 1400 ℃, keeping the temperature for 2 hours, naturally cooling the composite sol to normal temperature, washing the composite sol with absolute ethyl alcohol for 4 times, and putting the composite ceramsite in a baking oven at the temperature of 35 ℃ for 2 hours to prepare the composite ceramsite;
(2) The method comprises the following steps of (1) 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 5 hours at 4750r/min, then adding phosphorus pentachloride with the mass 0.7 times of that of the composite ceramsite, shearing for 5 hours, pouring into a mould at 50 ℃ for fixing for 5 hours, and drying at 85 ℃ for 24 hours to obtain a ceramsite concrete base material;
(3) Under the protection of argon at the temperature, chlorinated polypropylene with the molecular weight of 2000 and benzoic acid are mixed according to the mass ratio of 1:4, mixing, stirring for 15min at 500r/min, adding aluminum trichloride with the mass which is 0.02 times that of the chlorinated polypropylene, cooling to 2 ℃ at 3 ℃/min, and stirring for 8h at 700r/min to prepare the polypropylene-based benzoic acid; under the conditions of room temperature and argon protection, the mass ratio of the propenyl benzoic acid to the formamide is 1:0.7, mixing, stirring for 25min at 500r/min, then adding nano titanium dioxide with the mass 0.07 times of that of the propenyl benzoic acid, heating to 90 ℃ at 9.5 ℃/min, and continuously stirring for 3h to prepare the polypropylene benzoic acid formamide; under the conditions of room temperature and argon protection, placing a ceramsite concrete base material into a 4MPa closed container, pouring polypropylene-based benzoic acid formamide with the mass of 0.5 times of that of the ceramsite concrete base material, dropwise adding a sodium hydroxide solution with the mass fraction of 30% at 60 drops/min, regulating the pH value to 9, standing for 2 hours, and then, according to the 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 2450MHz and 800W microwave conditions, adding dimethyl sulfate with the mass of 0.02 times of that of the ceramsite concrete base material, continuing microwave treatment for 40min, demolding, putting into a reaction kettle with the pressure of 0.8MPa, heating to 670 ℃ at 10 ℃/min, carrying out heat preservation for 4h, heating to 1300 ℃, and carrying out heat preservation for 7h, thus obtaining the ceramsite concrete material.
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