CN113620686B - Preparation method of high-temperature-resistant nano heat-insulating mud - Google Patents

Preparation method of high-temperature-resistant nano heat-insulating mud Download PDF

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CN113620686B
CN113620686B CN202110924441.0A CN202110924441A CN113620686B CN 113620686 B CN113620686 B CN 113620686B CN 202110924441 A CN202110924441 A CN 202110924441A CN 113620686 B CN113620686 B CN 113620686B
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CN113620686A (en
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刘晓波
何沐
安烜熜
王子宁
张凡
李文静
刘瑾
杨洁颖
张昊
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Aerospace Research Institute of Materials and Processing Technology
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/24Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing alkyl, ammonium or metal silicates; containing silica sols
    • C04B28/26Silicates of the alkali metals
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/001Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing unburned clay
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/76Use at unusual temperatures, e.g. sub-zero
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    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/20Mortars, concrete or artificial stone characterised by specific physical values for the density
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    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/30Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
    • C04B2201/32Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/50Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength

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Abstract

The invention discloses a preparation method of high-temperature-resistant nano heat-insulating mud, belonging to the technical field of heat-insulating material preparation, and the method comprises the steps of weighing an inorganic nano powder composition and an inorganic fiber composition, and mixing to obtain a composition A; weighing the inorganic powder composition and ethanol, mixing and then ball-milling to obtain a composition B; weighing water, ethanol and an adhesive, and mixing to prepare a solution C; preparing a functional assistant solution D, wherein the solute phase of the functional assistant solution D is a composition of a surfactant, a preservative and an antistatic agent; and pouring the solution C into the composition A, stirring and mixing uniformly, then adding the composition B and the functional aid solution D, and stirring and mixing uniformly again to obtain the nano heat insulation mud. The invention can innoxiously prepare the high-temperature-resistant nano heat-insulating mud, and solves the problems of poor high-temperature resistance, toxic and harmful solvent system, complex use method and the like of the existing heat-insulating mud.

Description

Preparation method of high-temperature-resistant nano heat-insulating mud
Technical Field
The invention belongs to the technical field of heat insulation material preparation, and particularly relates to a preparation method of high-temperature-resistant nano heat insulation mud.
Background
The heat insulation materials are various and are classified from the material state, and comprise rigid heat insulation materials, flexible heat insulation materials and heat insulation coatings; including organic and inorganic insulation materials, depending on the material properties. With the continuous development of modern industry, the use scenes and application requirements of heat insulation materials tend to be diversified, and the original heat insulation material system and the preparation method thereof cannot meet the new requirements of the modern industry on heat insulation materials. For example, the demand of positions such as narrow and small space, complex structure dysmorphism piece, joint seam to thermal insulation material facing equipment, three kinds of thermal insulation materials all can't satisfy: the rigid heat insulation material needs to be realized by complex machining, so the cost is high; the flexible heat-insulating material does not have structural bearing capacity and has poor mechanical property; the heat-insulating coating is not thick enough and cannot be constructed in a narrow space.
The heat insulation mud serving as a novel heat insulation material has good plastic deformation capacity and good heat insulation performance, and has good development prospect in the future. However, the existing heat insulation mud product mainly comprises an organic silicon rubber system, has serious and insufficient comprehensive performance, and has the problems of poor high temperature resistance, toxic and harmful solvent system, complex use method and the like.
The published Chinese patent CN106830957A discloses a nano-scale microporous heat-insulating cement which uses a toxic and harmful anhydrous organic solvent, has higher pollution, uses resin as an organic adhesive component, is inevitably decomposed thoroughly at the temperature of over 600 ℃, loses strength along with the decomposition of the adhesive at high temperature, becomes loose powder and cannot be used at high temperature.
Disclosure of Invention
The invention aims to provide a preparation method of high-temperature-resistant nano heat-insulating mud, which is used for preparing the high-temperature-resistant nano heat-insulating mud in a harmless manner and solves the problems of poor high-temperature resistance, toxic and harmful solvent system, complex use method and the like of the existing heat-insulating mud.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of high-temperature-resistant nano heat-insulating mud comprises the following steps:
1) Weighing the inorganic nano powder composition and the inorganic fiber composition, and uniformly mixing at a high speed to obtain a composition A;
2) Weighing the inorganic powder composition and ethanol, mixing and then ball-milling to obtain a composition B;
3) Weighing water, ethanol and an adhesive, and mixing to prepare a solution C;
4) Preparing a functional assistant solution D, wherein the solute phase of the functional assistant solution D is a composition of a surfactant, a preservative and an antistatic agent;
5) And pouring the solution C into the composition A, stirring and mixing uniformly, then adding the composition B and the functional aid solution D, and stirring and mixing uniformly again to obtain the nano heat insulation mud.
Further, the mass ratio of the inorganic nano powder composition to the inorganic fiber composition is (5-10): 1.
Further, the inorganic nano powder composition comprises nano silicon dioxide, and also comprises any one or more of nano silicon carbide, nano chromium oxide, nano titanium dioxide and nano aluminum oxide; wherein the mass ratio of the nano silicon dioxide is not less than 40%.
Further, the inorganic fiber composition is ceramic fiber, and is specifically selected from one or more of quartz fiber, alumina fiber, zirconia fiber, mullite fiber, high silica fiber, glass fiber and silicon carbide fiber.
Further, the inorganic fiber composition comprises 1mm, 3mm, 5mm, 7mm and 9mm of inorganic fibers with different lengths, and the mass ratio of the inorganic fibers to each other is (1-2): 2-3): 8-10): 3-4): 1-3.
Further, after mixing in the step 2), ball milling is carried out for 2-8 hours at the speed of 100-400 r/min.
Further, the mass ratio of the ethanol to the inorganic powder composition is (2-10): 1.
Further, the inorganic powder composition is a composition of boron nitride nanosheets and mica flake powder in any proportion.
Furthermore, the mass ratio of the water, the ethanol and the adhesive is (90-100): 1-10): 5-10.
Further, the adhesive is selected from one of silicate, phosphate and clay, the silicate is preferably sodium silicate, and the phosphate is preferably aluminum phosphate.
Furthermore, the solvent phase of the functional assistant solution D is a composition prepared from ethanol and water according to the mass ratio of (8-10) to 1.
Further, the addition ratio of the solution C is calculated by the following formula:
solution C addition mass = (inorganic nano powder mass x (2.1-2.3) in composition a) + inorganic fiber mass x (0.2-0.5) in composition a)/(1-mass fraction of solution C);
the adding mass of the composition B is 5-10% of that of the composition A;
the addition mass of the solution D is 0.1-1% of the mass of the composition A.
The beneficial effects obtained by the invention are as follows:
1) In the preparation process, water and ethanol are used as solvent systems, and the water-based inorganic adhesive is used, so that the water-based inorganic adhesive is harmless to human bodies, does not relate to the use of harmful organic solvents such as esters, benzenes and aldehydes, and is green, safe and environment-friendly in the use process;
2) The prepared nanometer heat insulation mud can be formed into any shape, does not need to use a curing agent, can be cured by heating at normal temperature or 50-95 ℃, has simple use method, and is suitable for forming special-shaped heat insulation parts and keeping the surface of the special-shaped parts to keep warm and insulate heat along with the shape;
3) The density of the prepared nano heat insulation mud after curing is 0.4-0.8g/cm 3 Adjustable within a range, adjustable within a thermal conductivity coefficient range of 0.04-0.09W/(m.K), compression strength of more than 0.5MPa, temperature resistance of more than 800 ℃, excellent temperature resistance, heat insulation performance and mechanical property.
Drawings
FIG. 1 is a flow chart of the preparation of a high temperature resistant nano heat insulation mud.
Detailed Description
In order to make the aforementioned and other features and advantages of the invention more comprehensible, embodiments accompanied with figures are described in detail below.
The invention provides a preparation method of high-temperature-resistant nano heat-insulating mud, which comprises the following steps of:
1) And weighing the inorganic nano powder composition and the inorganic fiber composition, and uniformly mixing at a high speed to obtain the composition A. The mass ratio of the inorganic nanopowder composition to the inorganic fiber composition is (5-10): 1, and may be any ratio within the range, for example, 5. The inorganic nano powder composition comprises nano silicon dioxide, and also comprises any one or more of nano silicon carbide, nano chromium oxide, nano titanium dioxide and nano aluminum oxide; wherein the mass ratio of the nano silicon dioxide is not less than 40%. The inorganic fiber composition is one or more of ceramic fibers, and the ceramic fibers comprise quartz fibers, alumina fibers, zirconia fibers, mullite fibers, high silica fibers, glass fibers and silicon carbide fibers. The inorganic fiber composition comprises five inorganic fibers with different lengths of 1mm, 3mm, 5mm, 7mm and 9mm, and the mass ratio of the inorganic fibers to each other is (1-2) to (2-3) to (8-10) to (3-4) to (1-3), and can be any ratio in the range of 1.
2) The method comprises the following steps of weighing ethanol and an inorganic powder composition, wherein the inorganic powder composition can be a composition of boron nitride nanosheets and mica flake powders in any proportion, the mass ratio of the ethanol to the inorganic powder composition is (2-10): 1, and can be any proportion within the range, for example, the ratio of 2. Then, the mixture is mixed and ball milled, the ball milling speed is 100 to 400r/min (any value in the range, for example, 100r/min, 200r/min, 300r/min and 400 r/min), and the ball milling time is 2 to 8 hours (any value in the range, for example, 2 hours, 3 hours, 4 hours, 5 hours, 6 hours, 7 hours and 8 hours), so as to obtain the composition B.
3) The adhesive is one of silicate, phosphate and clay, the silicate is preferably sodium silicate, and the phosphate is preferably aluminum phosphate. The mass ratio of water, ethanol and the adhesive is (90-100): (1-10): (5-10), and can be any ratio within the range, for example, can be 90. The invention takes water and ethanol as solvent systems, uses water-based inorganic adhesive, is harmless to human body, does not relate to the use of harmful organic solvents such as esters, benzenes, aldehydes and the like, and has green, safe and environment-friendly use process.
4) Preparing a functional assistant solution D, wherein the solute phase of the functional assistant solution D is a composition of a surfactant, a preservative and an antistatic agent, and the solvent phase of the functional assistant solution D is a composition prepared by mixing ethanol and water according to a mass ratio of (8-10) to 1, and the ratio can be any ratio in the range, for example, 8.
5) And pouring the solution C into the composition A, stirring and mixing uniformly, then adding the composition B and the functional aid solution D, and stirring and mixing uniformly again to obtain the nano heat insulation mud. Wherein the adding proportion of the solution C is calculated by the following formula: solution C addition mass = (inorganic nano powder mass x (2.1-2.3) in composition a) + inorganic fiber mass x (0.2-0.5) in composition a)/(1-mass fraction of solution C); the added mass of the composition B is 5% to 10% of the added mass of the composition a, and may be any value within this range, for example, 5%, 6%, 7%, 8%, 9%, 10%; the added mass of the solution D may be 0.1% to 1% of the mass of the composition a, and may be any value within this range, for example, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1%.
The following are illustrative examples of the invention:
example 1
1) Weighing an inorganic nano powder composition and an inorganic fiber composition, wherein the inorganic nano powder composition comprises 60% of nano silicon carbide and 40% of nano silicon dioxide by mass, the inorganic fiber composition is quartz fiber, and the mass ratio of five materials with different lengths is 2.
2) Weighing an inorganic powder composition and ethanol, wherein the inorganic powder composition is a composition formed by mixing boron nitride nanosheets and mica flake powder according to a mass ratio of 1.
3) Weighing water, ethanol and sodium silicate serving as an adhesive, mixing the water, the ethanol and the sodium silicate in a mass ratio of 90;
4) Preparing a functional aid solution D, wherein the solute phase of the functional aid solution D is a composition of a surfactant, a preservative and an antistatic agent, and the solvent phase of the functional aid solution D is a composition prepared from ethanol and water according to a mass ratio of 8.
5) Solution C was poured into composition a, the added mass of solution C being calculated as: (the mass of the inorganic nanopowder in composition A. Times.2.1 + the mass of the inorganic fiber in composition A. Times.0.4) ÷ (1-mass fraction of solution C), wherein the mass of composition B added is 5% of the mass of composition A, and the mass of solution D added is 1% of the mass of composition A. And after stirring and mixing uniformly, adding the composition B and the functional assistant solution D, and stirring and mixing uniformly again to obtain the nano heat insulation mud.
The density of the high-temperature-resistant nano heat insulation mud prepared by the embodiment after curing is 0.7g/cm 3 The heat conductivity coefficient is 0.075W/(m.K), the compression strength is 2.5MPa, and the temperature resistance is 1300 ℃.
Examples 2-3 are identical to example 1 in the procedure except for the different conditions, and are detailed in table 1 below:
TABLE 1
Figure GDA0003843123510000041
Figure GDA0003843123510000051
A comparative example is set forth below, using a prior art manufacturing process, in contrast to example 3, with approximately the same procedure, with some differences, as detailed in Table 2 below:
TABLE 2
Figure GDA0003843123510000052
As can be seen from the above table, the comparative example is prepared by adding ethanol and adhesive and mixing to prepare solution C, no water is added, the adhesive is resin, and toxic and harmful anhydrous organic solvent is used, so that the pollution is higher. The effect of the embodiment shows that the compression strength is 1.0MPa, the temperature resistance is only 400 ℃, and when the temperature is above 400 ℃, the heat insulation mud begins to lose the strength and becomes loose and powder when the temperature is 600 ℃. In the preparation process, water and ethanol are used as solvent systems, the water-based inorganic adhesive is used, the preparation method is harmless to human bodies, harmful organic solvents such as esters, benzenes and aldehydes are not involved, and the use process is green, safe and environment-friendly. The compression strength is more than 0.5MPa, the temperature resistance is more than 800 ℃, and the temperature resistance, the heat insulation performance and the mechanical property are excellent.
Although the present invention has been described with reference to the above embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (4)

1. The preparation method of the high-temperature-resistant nano heat insulation mud is characterized by comprising the following steps of:
1) Weighing an inorganic nano powder composition and an inorganic fiber composition according to the mass ratio of (5-10) 1, wherein the inorganic nano powder composition comprises nano silicon dioxide and any one or more of nano silicon carbide, nano chromium oxide, nano titanium dioxide and nano aluminum oxide, and the mass ratio of the nano silicon dioxide is not lower than 40%; the inorganic fiber composition comprises 1mm, 3mm, 5mm, 7mm and 9mm of inorganic fibers with different lengths in the mass ratio of (1-2) to (2-3) to (8-10) to (3-4) to (1-3), and is uniformly mixed at a high speed to obtain a composition A;
2) Weighing ethanol and an inorganic powder composition according to the mass ratio of (2-10): 1, wherein the inorganic powder composition is a composition of boron nitride nanosheets and mica flake powder in any proportion, mixing and then ball-milling to obtain a composition B;
3) Weighing water, ethanol and an adhesive according to the mass ratio of (90-100) to (1-10) to (5-10), wherein the adhesive is selected from one of silicate, phosphate and clay, and mixing to prepare a solution C;
4) Preparing a functional assistant solution D, wherein the solute phase of the functional assistant solution D is a composition of a surfactant, a preservative and an antistatic agent, and the solvent phase of the functional assistant solution D is a composition prepared from ethanol and water according to a mass ratio of (8-10) to 1;
5) Pouring the solution C into the composition A, stirring and mixing uniformly, then adding the composition B and the functional assistant solution D, and stirring and mixing uniformly again to obtain the nano heat insulation mud;
wherein the addition proportion of the solution C is calculated by the following formula:
solution C addition mass = (inorganic nano powder mass x (2.1-2.3) in composition a) + inorganic fiber mass x (0.2-0.5) in composition a)/(1-mass fraction of solution C);
wherein the addition mass of the composition B is 5-10% of that of the composition A; the addition mass of the solution D is 0.1-1% of the mass of the composition A.
2. The method according to claim 1, wherein the inorganic fiber composition is a ceramic fiber, and is selected from one or more of quartz fiber, alumina fiber, zirconia fiber, mullite fiber, silica-rich fiber, glass fiber, and silicon carbide fiber.
3. The method of claim 1, wherein the ball milling in step 2) is performed at a speed of 100 to 400r/min for 2 to 8 hours after mixing.
4. The method of claim 1, wherein the silicate is sodium silicate and the phosphate is aluminum phosphate.
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CN106830957A (en) * 2017-03-10 2017-06-13 天津南极星隔热材料有限公司 A kind of nanometer level microporous heat-insulated clay
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