CN115772014A - Preparation method of heat-insulation ceramsite concrete material - Google Patents

Preparation method of heat-insulation ceramsite concrete material Download PDF

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CN115772014A
CN115772014A CN202211344496.5A CN202211344496A CN115772014A CN 115772014 A CN115772014 A CN 115772014A CN 202211344496 A CN202211344496 A CN 202211344496A CN 115772014 A CN115772014 A CN 115772014A
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mass
ceramsite
ceramsite concrete
mixing
stirring
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CN115772014B (en
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张皓
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Guangzhou Suifan Concrete Co ltd
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Abstract

The invention discloses a preparation method of a heat-insulation ceramsite concrete material, 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

Preparation method of heat-insulation ceramsite concrete material
Technical Field
The invention relates to the technical field of concrete, in particular to a preparation method of a heat-insulation ceramsite concrete material.
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 heat preservation direction, wherein ceramsite concrete is concrete prepared by replacing stones with ceramsite as concrete aggregate, is light and heat-preservation due to loose and porous structure, is light aggregate concrete, is also distinguished 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 polypropylene benzamide.
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 deionized water at the temperature of 60-80 ℃ in a mass ratio of 1:0.3:0.14:0.7:1.1 to 1:0.5:0.16:0.9:1.3, mixing, shearing for 4 to 6 hours at 4500 to 5000r/min, adding phosphorus pentachloride with the mass of 0.6 to 0.8 times of that of the composite ceramsite, shearing for 4 to 6 hours, pouring into a mold at 48 to 52 ℃, fixing for 4 to 6 hours, and then baking for 23 to 25hours at 80 to 90 ℃ 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 polypropylene benzoic acid formamide with the quality of 0.4-0.6 time of the ceramsite concrete base material, dropwise adding a sodium hydroxide solution with the mass fraction of 30% at a rate of 60 drops/min, adjusting the pH value to 9, standing for 1-3 h, and then mixing the components in a mass ratio of 1:8 to 1:12, adding zinc oxide and pyridine, wherein the mass of the zinc oxide is 0.01 to 0.016 times of that of the ceramsite concrete base material, performing ultrasonic treatment for 10 to 20min at 30 to 40kHz, performing microwave treatment for 15 to 25min under the microwave conditions of 2400 to 2500MHz and 700 to 900W, adding dimethyl sulfate with the mass of 0.01 to 0.03 time of that of the ceramsite concrete base material, performing microwave treatment for 30 to 50min, demolding, putting into a reaction kettle with the pressure of 0.7 to 0.9MPa, heating to 660 to 680 ℃ at the speed of 9 to 11 ℃/min, preserving heat for 2 to 6h, heating to 1200 to 1400 ℃ and preserving heat for 4 to 10h, and preparing the ceramsite concrete material.
Further, the preparation method of the composite ceramsite in the step (1) comprises the following steps: and (2) freezing the composite sol in a refrigerator at-4 to-2 ℃ for 47 to 49h, drying at 10 to 20Pa and at-50 to-40 ℃ for 47 to 49h, washing with absolute ethyl alcohol for 2 to 4 times, drying in a drying oven at 10 to 20Pa and at 19 to 21 ℃ for 1 to 3h, soaking in a nickel nitrate solution with the mass fraction of 10% and the mass fraction of 0.2 to 0.3 times that of the composite sol for 10 to 20h, taking out, placing in a reaction kettle at 0.7 to 0.9MPa, heating at 9 to 11 ℃/min to 710 ℃ and keeping the temperature for 1 to 3h, heating to 1300 to 1500 ℃, keeping the temperature for 1 to 3h, naturally cooling to the normal temperature, washing with absolute ethyl alcohol for 3 to 5 times, and placing in a drying oven at 30 to 40 ℃ for 1 to 3h to obtain the composite ceramsite.
Further, the preparation method of the composite sol comprises the following steps: under the protection of argon at the temperature of 80 to 90 ℃, trimethyl aluminate and deionized water are mixed according to the mass ratio of 1:7 to 1:9, stirring for 1 to 3 hours at 400 to 600r/min, dripping a nitric acid solution with the mass fraction of 11 to 13 percent, the mass of which is 0.2 to 0.3 times that of trimethyl aluminate, into the nitric acid solution at 40 to 60 drops/min, continuously stirring for 1 to 3 hours, adding silver with the mass of which is 0.01 to 0.03 times that of trimethyl aluminate, heating to 500 to 560 ℃ at 9 to 11 ℃/min, keeping the temperature for 8 to 10hours, cooling to 24 to 26 ℃ at 9 to 11 ℃/min, adding tetraphenyl silicate with the mass of which is 2 to 4 times that of trimethyl aluminate into the nitric acid solution, and (2) continuously dropwise adding ethanol with the mass of 8-16 times of that of the trimethyl aluminate, continuously stirring for 2-4h at the temperature of 60-80 ℃, adding ammonium hydroxide with the mass of 0.08-0.16 time of the trimethyl aluminate, continuously stirring for 10-20min, heating to 65-85 ℃ at the speed of 2-4 ℃/min, continuously stirring for 10-20min, continuously heating to 95-105 ℃, and stirring for 60-80min at the speed of 600-800r/min to prepare 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 to 1:0.8, stirring for 20 to 30min at 400 to 600r/min, then adding nano titanium dioxide with the mass of 0.06 to 0.08 times of that of the acrylic benzoic acid, heating to 80 to 100 ℃ at 9 to 10 ℃/min, and continuously stirring for 2 to 4h to prepare the polypropylene benzamide.
Further, the preparation method of the polyacrylic benzoic acid comprises the following steps: under the conditions of room temperature and argon protection, mixing chlorinated polypropylene and benzoic acid according to a mass ratio of 1:3 to 1:5, mixing, stirring for 10 to 20min at 400 to 600r/min, adding aluminum trichloride with the mass being 0.01 to 0.03 time that of polypropylene chloride, cooling to 0 to 4 ℃ at 2 to 4 ℃/min, and stirring for 7 to 9h at 600 to 800r/min to prepare the polyacrylic benzoic acid.
Further, the molecular weight of the chlorinated polypropylene is 1000 to 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 tetraphenyl silicate and the trimethyl aluminate react and crosslink to form silica aerogel and alumina, so that the heat-insulating property 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 present invention, the following examples are used for describing the method in detail, 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.
The flame retardant property is as follows: the flame retardance of the heat-insulating ceramsite concrete materials prepared in the same mass example 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 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 for fracture toughness 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, fishing 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 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) Under the conditions of room temperature and argon protection, chlorinated polypropylene with the molecular weight of 1000 and benzoic acid are mixed according to the mass ratio of 1:3, mixing, stirring at 400r/min for 10min, adding aluminum trichloride of which the mass is 0.01 time that of chlorinated polypropylene, cooling to 0 ℃ at 2 ℃/min, stirring at 600r/min for 7h, 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 for 20min at 400r/min, then adding nano titanium dioxide with the mass of 0.06 time of that of the propylene benzoic acid, heating to 80 ℃ at 9 ℃/min, and continuously stirring for 2h to prepare the polypropylene benzoic acid formamide; placing a ceramsite concrete base material into a 3MPa closed container at room temperature under the protection of argon, pouring polyacrylic benzoic acid formamide with the mass of 0.4 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 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; freezing the composite sol in a refrigerator at the temperature of-3 ℃ for 48h, drying at the temperature of 15Pa and-45 ℃ for 48h, washing with absolute ethyl alcohol for 3 times, drying in a drying oven at the temperature of 15Pa and 20 ℃ for 2h, soaking 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, fishing out, putting in 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 normal temperature, washing with absolute ethyl alcohol for 4 times, and drying in a drying oven at the temperature of 35 ℃ for 2h to prepare 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) Under the conditions of room temperature and argon protection, 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 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 mass ratio of the propylene benzoic acid to the formamide is 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 propylene benzoic acid, heating to 90 ℃ at 9.5 ℃/min, and continuing stirring for 3h to prepare the polypropylene benzamide; 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, demoulding, putting the mixture into a 0.8MPa reaction kettle, heating to 670 ℃ at 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 percent, the mass of which is 0.3 time that of trimethyl aluminate is added at 60 drops/min, continuously stirring for 3 hours, adding silver with the mass of which is 0.03 time 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 which is 4 times that of trimethyl aluminate, continuously dropwise adding ethanol with the mass of which is 16 times that of trimethyl aluminate, continuously stirring for 4 hours at 80 ℃, adding ammonium hydroxide with the mass of which is 0.16 time 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 prepare a 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 an 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, taking 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 an 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 being 0.8 time of that of the composite ceramsite, shearing for 6h, pouring the mixture into a mold at 52 ℃ for fixation for 6h, and drying at 90 ℃ for 25h to obtain a ceramsite concrete base material;
(3) Under the conditions of room temperature and argon protection, 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 at room temperature under the protection of argon, pouring polyacrylic benzoic acid formamide with the mass of 0.6 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 3 hours, and then mixing the components in a 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 the speed of 11 ℃/min, keeping the temperature for 6h, heating to 1400 ℃, and keeping the temperature 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, continuously stirring 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, continuously dropwise adding ethanol with the mass of 12 times of trimethyl aluminate, continuously stirring for 3h at 70 ℃, adding ammonium hydroxide with the mass of 0.12 time of trimethyl aluminate, continuously stirring for 15min, heating to 75 ℃ at 3 ℃/min, continuously stirring for 15min, heating to 100 ℃, stirring for 70min at 700r/min, and preparing 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 dipped 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, 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 percent, which is 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 dipped 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, 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) Under the conditions of room temperature and argon protection, 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 of which the mass is 0.02 time of 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, demoulding, putting the mixture into a 0.8MPa reaction kettle, heating to 670 ℃ at 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 time 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 with the mass of 0.02 time of that of the ceramsite concrete base material, continuing the microwave treatment for 40min, demoulding, putting the mixture into a reaction kettle with the pressure of 0.8MPa, heating to 670 ℃ at the speed of 10 ℃/min, keeping the temperature for 4h, heating to 1300 ℃, and keeping the temperature 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: under the conditions of room temperature and argon protection, 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 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 mass ratio of the propylene benzoic acid to the formamide is 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 193905DEST_PATH_IMAGE002
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; compared with the experimental data of the examples 1, 2 and 3 and the comparative example 1, the experiment data 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; the experimental data of the embodiments 1, 2, 3 and the comparative example 4 show that the heat-insulating ceramsite concrete material prepared by using phosphorus pentachloride can form a polypropylene network and aluminum nitride grains with cyclophosphazene as a center, and the prepared heat-insulating ceramsite concrete material has stronger flame retardant property and crack resistance; the experimental data of the embodiments 1, 2, 3 and the comparative example 5 show that when the polypropylene benzamide is used for preparing the thermal insulation ceramsite concrete material, a polypropylene network and aluminum nitride grains which take cyclophosphazene as a center can be formed, and the prepared thermal insulation ceramsite concrete material has strong flame retardant property and crack resistance; from the experimental data of the examples 1, 2, 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 strong 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 (1)

1. A preparation method of a heat-insulation 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, 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; 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 dipped 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, fished 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 normal temperature, then 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;
(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) Under the conditions of room temperature and argon protection, 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 of which the mass is 0.02 time of 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 mass ratio of the propylene benzoic acid to the formamide is 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 propylene benzoic acid, heating to 90 ℃ at 9.5 ℃/min, and continuing stirring for 3h to prepare the polypropylene benzamide; 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, demoulding, putting the mixture into a 0.8MPa reaction kettle, heating to 670 ℃ at 10 ℃/min, carrying out heat preservation for 4h, heating to 1300 ℃, and carrying out heat preservation for 7h to prepare the ceramsite concrete material.
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