CN113683389A - Method for producing silica aerogel felt by repeatedly utilizing supercritical waste liquid - Google Patents
Method for producing silica aerogel felt by repeatedly utilizing supercritical waste liquid Download PDFInfo
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- CN113683389A CN113683389A CN202111129801.4A CN202111129801A CN113683389A CN 113683389 A CN113683389 A CN 113683389A CN 202111129801 A CN202111129801 A CN 202111129801A CN 113683389 A CN113683389 A CN 113683389A
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B30/00—Compositions for artificial stone, not containing binders
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/02—Granular materials, e.g. microballoons
- C04B14/04—Silica-rich materials; Silicates
- C04B14/06—Quartz; Sand
- C04B14/064—Silica aerogel
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- C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
- C04B22/002—Water
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, 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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Abstract
The invention belongs to the field of waste liquid recycling, and discloses a method for producing a silica aerogel felt by repeatedly utilizing supercritical waste liquid. According to the invention, the hydrolysis and polycondensation reactions of the silicon source are respectively carried out in different reactors, so that the condition of inconsistent gel degree caused by the simultaneous hydrolysis and polycondensation is avoided, and the phenomenon that firmer network microstructure solids generated by the simultaneous hydrolysis and polycondensation of the silicon source are attached to the inner wall of the reactor is avoided, thereby shortening the service life of the equipment; meanwhile, the recycled supercritical waste liquid is recycled in the silica sol-gel process through gasification, so that the recycling of the waste liquid is ensured, resources are reasonably utilized, and the cost is saved.
Description
Technical Field
The invention belongs to the field of waste liquid recycling, and particularly relates to a method for producing a silica aerogel felt by repeatedly utilizing supercritical waste liquid.
Background
Aerogels are highly porous materials composed of nanoparticles, and have high porosity, specific surface area, and low thermal conductivity, thereby drawing attention as efficient heat insulating materials, sound insulating materials, and the like. However, aerogel blankets have not been widely used in the market despite their excellent thermal insulation properties when compared to conventional insulation materials due to their high production cost. The product price of aerogel blankets is relatively higher than that of other insulation materials due to the expensive raw materials, complicated manufacturing processes, and the cost of disposing of the large amount of waste liquid generated during the manufacturing process.
The method of reducing the cost by changing the raw material or changing the production process among the above price-increasing factors directly affects the quality of the product, and thus is not suitable for application, and the simplest method of reducing the cost is to reuse the waste liquid generated in the production process.
On the other hand, in the prior art, the preparation process of the aerogel is generally as follows: injecting a liquid-phase silicon source substance and other raw materials in a certain proportion into a reactor, uniformly mixing and stirring at normal temperature, adding a certain solution as a catalyst to fully hydrolyze the liquid-phase silicon source substance, and adding a proper amount of another liquid-phase catalyst after a certain time. And then, spraying the sol onto various prepared fiber base materials through a dipping machine, standing and aging the prepared gel felt for several hours to ensure that the gel is full and a firmer network microstructure is formed. In the above process, the sol and the gel are produced almost simultaneously, which means that the raw materials undergo hydrolysis and polycondensation simultaneously, the sol is in a solid-liquid mixture state, and the sol undergoing hydrolysis-polycondensation reaction is sprayed on various fiber base materials, so that the impregnation is not uniform, the combination of the aerogel and the base materials is not uniform enough, and the uniformity of the heat conductivity coefficient of the final product is poor. And because the two production processes of sol and gel are carried out in the same reactor, some firmer network microstructure solids are attached to the inner wall of the reactor, and the normal operation of equipment can be influenced after long-term accumulation.
Therefore, the gas-phase catalyst for the gel preparation process by using the supercritical waste liquid is used, the hydrolysis and polycondensation reaction of the silicon source are respectively carried out, the supercritical waste liquid can be reused, the cost is reduced, and the aerogel with excellent performance can be prepared.
Disclosure of Invention
The invention aims to provide a method for producing a silica aerogel felt by repeatedly utilizing supercritical waste liquid, which repeatedly utilizes the supercritical waste liquid generated in the supercritical drying process of silica wet gel, and repeatedly utilizes the recovered supercritical waste liquid in the silica sol-gel process through gasification.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for producing silica aerogel felt by repeatedly utilizing supercritical waste liquid comprises the following steps:
(1) recovering supercritical waste liquid generated in the supercritical drying process of the wet silica gel;
(2) mixing a silicon source, ethanol and water according to the ratio of the silicon source to the ethanol to the water = 1: 2-60: 1-30 to obtain silicon dioxide sol;
(3) soaking the fiber material in the silica sol obtained in the step (2) for 8-24h to obtain a sol composite material;
(4) transferring the sol composite material impregnated in the step (3) into a gel reactor, gasifying the supercritical waste liquid obtained in the step (1), introducing the gasified supercritical waste liquid into the gel reactor, and performing catalytic gelling reaction to obtain a gel composite material;
(5) and (5) carrying out supercritical drying on the gel composite material obtained in the step (4) to obtain the silica aerogel felt.
The silicon source is one or more than two of ethyl orthosilicate, methyl orthosilicate, butyl orthosilicate, isopropyl orthosilicate or alkyl alkoxy silane.
Preferably, the supercritical waste liquid obtained in step (1) contains water, organic solvent and ammonium ion NH4 +。
Preferably, the process of distilling the supercritical waste liquid after the supercritical waste liquid is recovered in the step (1); the distillation temperature is 70-80 ℃.
Preferably, the alkylalkoxysilane includes one or more of methyltrimethoxysilane, dimethyldimethoxysilane, methyltriethoxysilane, dimethyldiethoxysilane, vinyltriethoxysilane, propyltrimethoxysilane, or propyltriethoxysilane.
Preferably, the fiber material is a fiber batt, a fiber mat, a fiber roll; the fiber is one of pre-oxidized fiber, glass fiber, aluminum silicate fiber, quartz fiber, high silica fiber, carbon fiber, mullite fiber, basalt fiber, silicon carbide fiber, alumina fiber and boron nitride fiber.
Preferably, the supercritical waste liquid is gasified and then introduced into the sol composite material to ensure that the pH value of the sol composite material is 7-10.
Preferably, the gasification process in step (4) is to place the supercritical waste liquid in a steam generator to prepare a gas-phase gel catalyst, and introduce the generated gas into a gel reactor to perform a catalytic gelling reaction.
Preferably, an aging process is further included before the gel composite material is dried in the step (5), specifically, the gel composite material is aged for 8-24 hours at room temperature or at 30-60 ℃.
Preferably, a hydrophobization treatment process is further included before the gel composite material is dried in the step (5), specifically, the gel composite material is placed in an absolute ethanol solution containing 0.2-10% of a hydrophobization agent by volume fraction and is kept standing at room temperature for 1-24h, and the hydrophobization agent is one or two of hexamethyldisilazane or trimethoxymethylsilane.
Preferably, a solvent replacement process is further included before the gel composite is dried in the step (5), specifically, the silica wet gel sheet is placed in absolute ethyl alcohol for solvent replacement, the number of times of replacement is 1-4, and the time of each replacement is 2-12 hours.
Preferably, in the preparation process, after the supercritical drying in the step (5), the supercritical waste liquid is recycled and used in the sol-gel process of the silica aerogel.
The silica aerogel felt produced by using the supercritical waste liquid is obtained by the preparation method.
Has the advantages that:
based on the principle of gas phase catalysis, the waste liquid generated in the supercritical drying process is placed in a steam generator to prepare a gas phase gel catalyst in a gasification mode, and then the gas phase gel catalyst is introduced into a silica sol composite material to carry out catalytic gel reaction, so that the silica aerogel felt with good heat insulation performance is prepared.
The method provided by the invention can be used for repeatedly utilizing the supercritical waste liquid generated in the supercritical drying process, and repeatedly utilizing the recovered supercritical waste liquid in the silica sol-gel process through gasification, so that the reutilization of the waste liquid is ensured, the resources are reasonably utilized, and the cost is saved.
When the method provided by the invention is used for preparing the aerogel composite material, hydrolysis and polycondensation of the silicon source can be respectively carried out in different reactors, so that the condition that the gel degree is inconsistent because hydrolysis and polycondensation are carried out simultaneously is avoided, and firmer network microstructure solids generated by simultaneous hydrolysis and polycondensation of the silicon source are prevented from being attached to the inner wall of the reactor, thereby shortening the service life of equipment.
The preparation process provided by the invention does not need additional investment in equipment, is simple and economical in preparation process, and is beneficial to providing new improvement ideas and directions for the preparation process of the aerogel felt.
Detailed Description
The present invention will be further described with reference to the following specific examples. It should be understood that the following examples are illustrative only and are not intended to limit the scope of the present invention.
Example 1:
(1) recovering supercritical waste liquid generated in the supercritical drying process of the wet silica gel;
(2) mixing a silicon source, ethanol and water according to the ratio of the silicon source to the ethanol to the water = 1: 6: 2 to obtain silicon dioxide sol;
(3) soaking the fiber material in the silica sol obtained in the step (2) for 16 hours to obtain a sol composite material;
(4) transferring the sol composite material impregnated in the step (3) into a gel reactor, gasifying the supercritical waste liquid obtained in the step (1), introducing the gasified supercritical waste liquid into the gel reactor, and performing catalytic gelling reaction to obtain a gel composite material;
(5) and (5) carrying out supercritical drying on the gel composite material obtained in the step (4) to obtain the silica aerogel felt.
The supercritical waste liquid in the step (1) contains water, organic solvent and ammonium ions (NH)4 +) The organic solvent is mainly ethanol.
The silicon source is tetraethoxysilane; the fiber material is a glass fiber roll.
And gasifying the supercritical waste liquid, and introducing the sol composite material to enable the pH value of the sol composite material to be 8.
And (4) putting the supercritical waste liquid into a steam generator to prepare a gas-phase gel catalyst in the gasification process, and introducing the generated gas into a gel reactor to perform a catalytic gelling reaction.
The silica aerogel felt prepared by the preparation method.
The silica aerogel blanket obtained in this example had a thermal conductivity of 0.02 w/(m.cndot.).
Example 2:
(1) recovering supercritical waste liquid generated in the supercritical drying process of the wet silica gel;
(2) mixing a silicon source, ethanol and water according to the ratio of the silicon source to the ethanol to the water = 1: 30: 10 to obtain silica sol;
(3) soaking the fiber material in the silica sol obtained in the step (2) for 20 hours to obtain a sol composite material;
(4) transferring the sol composite material impregnated in the step (3) into a gel reactor, gasifying the supercritical waste liquid obtained in the step (1), introducing the gasified supercritical waste liquid into the gel reactor, and performing catalytic gelling reaction to obtain a gel composite material;
(5) aging: aging the gel composite material obtained in the step (4) for 16h at the temperature of 40 ℃;
(6) and (5) carrying out supercritical drying on the gel composite material obtained in the step (5) to obtain the silica aerogel felt.
The supercritical waste liquid in the step (1) contains water, organic solvent and ammonium ions (NH)4 +) The organic solvent is mainly ethanol.
The silicon source is methyl trimethoxy silane; the fiber material is an aluminum silicate fiber pad.
And gasifying the supercritical waste liquid, and introducing the sol composite material to enable the pH value of the sol composite material to be 7.
And (4) putting the supercritical waste liquid into a steam generator to prepare a gas-phase gel catalyst in the gasification process, and introducing the generated gas into a gel reactor to perform a catalytic gelling reaction.
The silica aerogel felt prepared by the preparation method.
The silica aerogel blanket obtained in this example had a thermal conductivity of 0.018 w/(m.cndot.).
Example 3:
(1) recovering supercritical waste liquid generated in the supercritical drying process of the wet silica gel;
(2) mixing a silicon source, ethanol and water according to the ratio of the silicon source to the ethanol to the water = 1: 8: 3 to obtain silica sol;
(3) soaking the fiber material in the silica sol obtained in the step (2) for 20 hours to obtain a sol composite material;
(4) transferring the sol composite material impregnated in the step (3) into a gel reactor, gasifying the supercritical waste liquid obtained in the step (1), introducing the gasified supercritical waste liquid into the gel reactor, and performing catalytic gelling reaction to obtain a gel composite material;
(5) and (3) hydrophobization treatment: placing the gel composite material obtained in the step (4) in an absolute ethyl alcohol solution containing a hydrophobization reagent with the volume fraction of 8%, and standing for 6 hours at room temperature;
(6) and (5) carrying out supercritical drying on the gel composite material obtained in the step (5) to obtain the silica aerogel felt.
The supercritical waste liquid in the step (1) contains water, organic solvent and ammonium ions (NH)4 +) The organic solvent is mainly ethanol.
The silicon source is tetraethoxysilane; the fiber material is a glass fiber mat.
And gasifying the supercritical waste liquid, and introducing the sol composite material to enable the pH value of the sol composite material to be 9.
And (4) putting the supercritical waste liquid into a steam generator to prepare a gas-phase gel catalyst in the gasification process, and introducing the generated gas into a gel reactor to perform a catalytic gelling reaction.
The hydrophobizing agent is hexamethyldisiloxane.
The silica aerogel felt prepared by the preparation method.
The silica aerogel felt obtained in the embodiment has a thermal conductivity of 0.019 w/(m.DEG C).
Example 4:
(1) recovering supercritical waste liquid generated in the supercritical drying process of the wet silica gel;
(2) after the supercritical waste liquid is recovered, the process of distilling the supercritical waste liquid is also included; the temperature of the distillation was 76 ℃.
(3) Mixing a silicon source, ethanol and water according to the ratio of the silicon source to the ethanol to the water = 1: 10: 6 to obtain silica sol;
(4) soaking the fiber material in the silica sol obtained in the step (3) for 18 hours to obtain a sol composite material;
(5) transferring the sol composite material impregnated in the step (4) into a gel reactor, gasifying the supercritical waste liquid obtained in the step (1), introducing the gasified supercritical waste liquid into the gel reactor, and performing catalytic gelling reaction to obtain a gel composite material;
(6) and (3) hydrophobization treatment: placing the gel composite material obtained in the step (5) in an absolute ethyl alcohol solution containing a hydrophobization reagent with the volume fraction of 8%, and standing at room temperature for 12 hours;
(7) and (5) performing supercritical drying on the gel composite material obtained in the step (6) to obtain the silica aerogel felt.
The supercritical waste liquid in the step (1) contains water, organic solvent and ammonium ions (NH)4 +) The organic solvent is mainly ethanol.
The silicon source is tetraethoxysilane; the fiber material is an aluminum silicate fiber pad.
And gasifying the supercritical waste liquid, and introducing the sol composite material to enable the pH value of the sol composite material to be 8.
And (4) putting the supercritical waste liquid into a steam generator to prepare a gas-phase gel catalyst in the gasification process, and introducing the generated gas into a gel reactor to perform a catalytic gelling reaction.
The hydrophobization reagent is trimethylchlorosilane.
The silica aerogel felt prepared by the preparation method.
The silica aerogel blanket obtained in the example had a thermal conductivity of 0.021 w/(m.cndot.).
Example 5
The difference from the example 3 is that the method further comprises the step of placing the gel composite material in absolute ethyl alcohol for solvent replacement for 3 times, wherein each time is 10 hours, before the supercritical drying in the step (6).
The silica aerogel felt prepared by the preparation method.
The silica aerogel blanket obtained in the example had a thermal conductivity of 0.019 w/(m.DEG.C.).
Claims (10)
1. A method for producing silica aerogel felt by recycling supercritical waste liquid is characterized in that the supercritical waste liquid generated in the supercritical drying process of silica wet gel is recycled, and the recycled supercritical waste liquid is recycled in the silica sol-gel process through gasification;
the method comprises the following specific steps:
(1) recovering supercritical waste liquid generated in the supercritical drying process of the wet silica gel;
(2) mixing a silicon source, ethanol and water according to the ratio of the silicon source to the ethanol to the water = 1: 2-60: 1-30 to obtain silicon dioxide sol;
(3) soaking the fiber material in the silica sol obtained in the step (2) for 8-24h to obtain a sol composite material;
(4) transferring the sol composite material impregnated in the step (3) into a gel reactor, gasifying the supercritical waste liquid obtained in the step (1), introducing the gasified supercritical waste liquid into the gel reactor, and performing catalytic gelling reaction to obtain a gel composite material;
(5) carrying out supercritical drying on the gel composite material obtained in the step (4) to obtain a silicon dioxide aerogel felt;
the silicon source is one or more than two of ethyl orthosilicate, methyl orthosilicate, butyl orthosilicate, isopropyl orthosilicate or alkyl alkoxy silane.
2. The method for producing the silica aerogel felt by recycling the supercritical waste liquid as claimed in claim 1, wherein the method comprises the following steps: the supercritical waste liquid in the step (1) contains water, organic solvent and ammonium ion NH4 +。
3. The method for producing the silica aerogel felt by recycling the supercritical waste liquid as claimed in claim 1, wherein the method comprises the following steps: after the supercritical waste liquid in the step (1) is recovered, the process of distilling the supercritical waste liquid is also included; the distillation temperature is 70-80 ℃.
4. The method for producing the silica aerogel felt by recycling the supercritical waste liquid as claimed in claim 1, wherein the method comprises the following steps: the alkyl alkoxy silane comprises one or more than two of methyl trimethoxy silane, dimethyl dimethoxy silane, methyl triethoxy silane, dimethyl diethoxy silane, vinyl triethoxy silane, propyl trimethoxy silane or propyl triethoxy silane.
5. The method for producing the silica aerogel felt by recycling the supercritical waste liquid as claimed in claim 1, wherein the method comprises the following steps: the fiber material is fiber batting, fiber mats and fiber coiled materials; the fiber is one of pre-oxidized fiber, glass fiber, aluminum silicate fiber, quartz fiber, high silica fiber, carbon fiber, mullite fiber, basalt fiber, silicon carbide fiber, alumina fiber and boron nitride fiber.
6. The method for producing the silica aerogel felt by recycling the supercritical waste liquid as claimed in claim 1, wherein the method comprises the following steps: and gasifying the supercritical waste liquid, and introducing the sol composite material to ensure that the pH value of the sol composite material is 7-10.
7. The method for producing the silica aerogel felt by recycling the supercritical waste liquid as claimed in claim 1, wherein the method comprises the following steps: and (4) putting the supercritical waste liquid into a steam generator to prepare a gas-phase gel catalyst in the gasification process, and introducing the generated gas into a gel reactor to perform a catalytic gelling reaction.
8. The method for producing the silica aerogel felt by recycling the supercritical waste liquid as claimed in claim 1, wherein the method comprises the following steps: and (3) before drying the gel composite material in the step (5), an aging process is also included, and specifically, the gel composite material is subjected to aging treatment for 8-24h at room temperature or under the condition of heating at 30-60 ℃.
9. The method for producing the silica aerogel felt by recycling the supercritical waste liquid as claimed in claim 1, wherein the method comprises the following steps: and (3) before the gel composite material is dried in the step (5), a hydrophobization treatment process is also included, specifically, the gel composite material is placed in an absolute ethyl alcohol solution containing 0.2-10% of a hydrophobization reagent in volume fraction, and is kept standing for 1-24h at room temperature.
10. The silica aerogel blanket produced by using the supercritical waste liquid prepared by the method of any one of claims 1 to 9.
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