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CN114804817A - Preparation method of efficient aerogel thermal insulation material - Google Patents

Preparation method of efficient aerogel thermal insulation material Download PDF

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Publication number
CN114804817A
CN114804817A CN202210374240.2A CN202210374240A CN114804817A CN 114804817 A CN114804817 A CN 114804817A CN 202210374240 A CN202210374240 A CN 202210374240A CN 114804817 A CN114804817 A CN 114804817A
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CN
China
Prior art keywords
preparation
thermal insulation
insulation material
fiber mixture
aerogel thermal
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CN202210374240.2A
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Chinese (zh)
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CN114804817B (en
Inventor
郑智宏
张静云
陈建文
程璇
武杰
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Xiamen Zhongchuang Environmental Protection Technology Co ltd
Xiamen University
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Xiamen Zhongchuang Environmental Protection Technology Co ltd
Xiamen University
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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
    • C04B30/00Compositions for artificial stone, not containing binders
    • C04B30/02Compositions for artificial stone, not containing binders containing fibrous materials
    • 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
    • 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
    • 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Silicon Compounds (AREA)

Abstract

The invention discloses a preparation method of a high-efficiency aerogel thermal insulation material, which comprises the steps of taking a waste polytetrafluoroethylene and polyphenylene sulfide fiber blending filter bag as a raw material, cleaning, cutting and opening the raw material to obtain a flocculent fiber mixture, and then soaking the flocculent fiber mixture in an oxalic acid solution and a sodium hypochlorite solution in sequence, washing the flocculent fiber mixture with water and drying the flocculent fiber mixture in the sun; then mixing and uniformly stirring methyl triethoxysilane, distilled water, absolute ethyl alcohol and ammonia water to obtain a mixed solution, pouring the mixed solution into a mold filled with a fiber mixture, and carrying out aging and drying treatment to obtain the aerogel thermal insulation material; wherein, calculated by volume ratio, the methyl triethoxysilane: distilled water: the absolute ethyl alcohol is 1 (2-3) to (2-3), ammonia water: the methyltriethoxysilane is 1 (20-30). The invention solves the problems that the waste blended filter bag is difficult to treat and easy to cause environmental pollution, realizes the reutilization and harmless treatment of resources, and enhances the mechanical property of the aerogel so as to prepare the high-efficiency aerogel thermal insulation material.

Description

Preparation method of efficient aerogel thermal insulation material
Technical Field
The invention relates to the technical field of environment-friendly materials, in particular to a preparation method of an efficient aerogel thermal insulation material.
Background
At present, a Polytetrafluoroethylene (PTFE) and polyphenylene sulfide (PPS) fiber blended filter bag is one of the common filter bag materials of a bag type dust collector/electric bag dust collector of a coal-fired power plant. The service life of the filter bag made of the material in a bag type dust collector/electric bag dust collector of a coal-fired power plant is normally 3-5 years, and the replaced old filter bag is generally treated by burning or landfill. Due to the large difference of the performances of the polytetrafluoroethylene and the polyphenylene sulfide, particularly the different melting points (the melting points of the polytetrafluoroethylene and the polyphenylene sulfide are 327 ℃ and 285 ℃ respectively), the polytetrafluoroethylene cannot be remelted for granulation and use, and meanwhile, the polytetrafluoroethylene is easy to decompose into gaseous fluorine-containing compounds under the high-temperature condition, most of decomposed substances are toxic substances, and the polytetrafluoroethylene is unsuitable in an incineration treatment mode, so that the environment is easily polluted, and the human health is easily damaged.
The silica aerogel is a solid phase particle, has a continuous and irregular nano porous network structure, has the characteristics of low density, very low heat conductivity coefficient, super hydrophobicity and the like, can be used as a light and efficient heat insulation material, but has the problems of poor mechanical property and easy fragmentation.
Disclosure of Invention
The invention aims to provide a preparation method of an efficient aerogel thermal insulation material, which utilizes waste polytetrafluoroethylene and polyphenylene sulfide fiber blended filter bags as raw materials to prepare an aerogel material with higher mechanical property, and realizes resource reutilization and harmless treatment of the waste filter bags.
In order to achieve the above purpose, the solution of the invention is:
a preparation method of a high-efficiency aerogel thermal insulation material comprises the following steps:
step 1, preliminary cleaning
Washing the waste blending filter bag by water and airing, wherein the blending filter bag is formed by blending polytetrafluoroethylene and polyphenylene sulfide fibers;
step 2, cutting and opening
Cutting and opening the blending filter bag to obtain a flocculent fiber mixture;
step 3, chemical cleaning
Soaking the fiber mixture in oxalic acid solution, washing with distilled water and drying in the sun; soaking the fiber mixture in sodium hypochlorite solution, and washing with distilled water and drying in the sun;
step 4, preparing the material
Mixing and uniformly stirring methyl triethoxysilane, distilled water, absolute ethyl alcohol and ammonia water to obtain a mixed solution, pouring the mixed solution into a mold filled with a fiber mixture, and performing aging and drying treatment to obtain an aerogel thermal insulation material; wherein, calculated by volume ratio, the methyl triethoxysilane: distilled water: the absolute ethyl alcohol is 1 (2-3) to (2-3), ammonia water: the methyltriethoxysilane is 1 (20-30).
In the step 2, the blended filter bag is cut into strips with the width of 5-10cm, and the strips are opened by a cloth opener to obtain a flocculent fiber mixture.
In the step 3, the fiber mixture is soaked in oxalic acid solution with the mass fraction of 10-20% and sodium hypochlorite solution with the mass fraction of 5.5-10% for 12-24 h.
In the step 4, the methyltriethoxysilane and the distilled water are mixed and stirred, and then the absolute ethyl alcohol and the ammonia water are poured for mixing and stirring.
In the step 4, the molar concentration of the ammonia water is 10 mol/L.
In the step 4, the aging temperature is 55-65 ℃, and the drying temperature is 80-100 ℃.
In the step 4, the aging time is 24-48h, and the drying time is 12-24 h.
In the step 4, the filling rate of the fiber mixture in the aerogel thermal insulation material is 5-20%.
In the step 4, the mixed solution is poured into a mould filled with the fiber mixture, then is kept stand for 30-60min, when the mixed solution is changed from colorless to turbid, absolute ethyl alcohol which is 2-4cm higher than the liquid level of the mould is poured into the mould, the mould is sealed for aging treatment, and after aging, the mould is opened, the mould is sealed and then is dried.
By adopting the technical scheme, the problem that a flexible user is difficult to recycle and treat the waste polytetrafluoroethylene and polyphenylene sulfide fiber blended filter bag is solved, the resource recycling and the harmless treatment of the waste filter bag can be realized, meanwhile, a flocculent fiber mixture is obtained by treating the polytetrafluoroethylene and polyphenylene sulfide blended filter bag through a series of cleaning processes and is used for enhancing the aerogel, the mechanical property of the aerogel can be effectively improved, and the efficient aerogel thermal insulation material is prepared.
Detailed Description
In order to further explain the technical solution of the present invention, the present invention is explained in detail by the following specific examples.
The invention discloses a preparation method of an efficient aerogel thermal insulation material, which comprises the following steps:
step 1, preliminary cleaning
Washing the waste blending filter bag by water and drying, wherein the blending filter bag is formed by blending polytetrafluoroethylene and polyphenylene sulfide fibers;
step 2, cutting and opening
Cutting and opening the blending filter bag to obtain a flocculent fiber mixture;
step 3, chemical cleaning
Soaking the fiber mixture in oxalic acid solution, washing with distilled water and drying in the sun; soaking the fiber mixture in sodium hypochlorite solution, and washing with distilled water and drying in the sun;
step 4, preparing the material
Mixing and uniformly stirring Methyl Triethoxysilane (MTES), distilled water, absolute ethyl alcohol and ammonia water to obtain a mixed solution, pouring the mixed solution into a mold filled with a fiber mixture, and performing aging and drying treatment to obtain an aerogel thermal insulation material; wherein, calculated by volume ratio, the methyl triethoxysilane: distilled water: the absolute ethyl alcohol is 1 (2-3) to (2-3), ammonia water: the methyltriethoxysilane is 1 (20-30).
In the step 2, the blended filter bag is cut into strips with the width of 5-10cm, and the strips are opened by a cloth opener to obtain a flocculent fiber mixture.
In the step 3, the fiber mixture is soaked in oxalic acid solution with the mass fraction of 10-20% and sodium hypochlorite solution with the mass fraction of 5.5-10% for 12-24h, and the heat conduction coefficient of the finally cleaned fiber mixture is 0.09-0.15W/m.k.
In the step 4, the methyltriethoxysilane and the distilled water are mixed and stirred, and then the absolute ethyl alcohol and the ammonia water are poured for mixing and stirring.
In the step 4, the molar concentration of the ammonia water is 10 mol/L.
In the step 4, the aging temperature is 55-65 ℃, and the drying temperature is 80-100 ℃.
Further, in the step 4, the aging time is 24-48h, and the drying time is 12-24 h.
In the step 4, the filling rate of the fiber mixture in the aerogel thermal insulation material is 5-20%.
In the step 4, the mixed solution is poured into a mould filled with the fiber mixture, then is stood for 30-60min, when the mixed solution is changed from colorless to turbid, absolute ethyl alcohol which is 2-4cm higher than the liquid level of the mould is poured into the mould, the mould is sealed for aging treatment, and after aging, the mould is opened, the mould is sealed and then is dried.
Through the scheme, the problem that a flexible user is difficult to recycle and treat the waste polytetrafluoroethylene and polyphenylene sulfide fiber blended filter bag is solved, the resource recycling and the harmless treatment of the waste filter bag can be realized, and meanwhile, a flocculent fiber mixture is obtained by treating the polytetrafluoroethylene and polyphenylene sulfide blended filter bag through a series of cleaning processes and is used for enhancing the aerogel, so that the mechanical property of the aerogel can be effectively improved, and the efficient aerogel thermal insulation material is prepared.
Specific embodiments of the present invention are shown below. Test materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
(1) Preliminarily cleaning and airing the waste polytetrafluoroethylene and polyphenylene sulfide blended filter bag by using water, then shearing the filter bag into strips with the width of 5-10cm, and opening the strips by using a cloth opener to obtain a flocculent fiber mixture;
(2) weighing 50g of analytically pure oxalic acid solid by using a beaker, dissolving the solid by using distilled water and pouring the solid into a 500ml volumetric flask, washing the beaker by using the distilled water, transferring the washing liquid into the volumetric flask, adding the distilled water to the position of a scale mark of the empty volumetric flask, and uniformly mixing the solid for later use; measuring 50ml of analytically pure sodium hypochlorite solution by using a measuring cylinder, pouring the solution into a 500ml volumetric flask, washing the measuring cylinder by using distilled water, transferring the washing solution into the volumetric flask, adding distilled water to the position of a scale mark of the volumetric flask, and uniformly mixing for later use; weighing 8.4263g of flocculent fiber mixture, soaking in 250ml of prepared oxalic acid solution for 24h, washing with distilled water, drying in the air, soaking in 250ml of prepared sodium hypochlorite solution for 24h, washing with distilled water, and drying in the air;
(3) respectively measuring 11ml of methyltriethoxysilane solution and 20ml of distilled water by using a measuring cylinder, mixing and stirring for 3 hours, adding 20ml of absolute ethyl alcohol and 0.48ml of ammonia water, uniformly stirring to obtain a mixed solution, measuring 20ml of the mixed solution, pouring the mixed solution into a glass mold filled with 0.0804g of fiber mixture, standing for 30 minutes, pouring absolute ethyl alcohol with the height of 2cm higher than the liquid level, sealing by using a preservative film, putting the mixed solution into a 55 ℃ oven for aging for 48 hours, uncovering the seal, putting the mixed solution into an 80 ℃ oven for drying for 24 hours to obtain the high-efficiency aerogel heat-insulating material, and testing that the heat conduction coefficient is 0.04840W/m.k, the density is 0.1316g/m3, and the resilience is 97.01%.
The proportion in the above embodiment is as follows: 0.0804g of the fiber mixture, 11ml of methyltriethoxysilane solution, 20ml of distilled water, 20ml of absolute ethanol, and 0.48ml of concentrated ammonia water.
The above embodiments are not intended to limit the form and style of the present invention, and any suitable changes or modifications made by those skilled in the art should be considered as not departing from the scope of the present invention.

Claims (9)

1. The preparation method of the high-efficiency aerogel thermal insulation material is characterized by comprising the following steps of:
step 1, preliminary cleaning
Washing the waste blending filter bag by water and airing, wherein the blending filter bag is formed by blending polytetrafluoroethylene and polyphenylene sulfide fibers;
step 2, cutting and opening
Cutting and opening the blending filter bag to obtain a flocculent fiber mixture;
step 3, chemical cleaning
Soaking the fiber mixture in oxalic acid solution, washing with distilled water and drying in the sun; soaking the fiber mixture in sodium hypochlorite solution, and washing with distilled water and drying in the sun;
step 4, preparing the material
Mixing and uniformly stirring methyl triethoxysilane, distilled water, absolute ethyl alcohol and ammonia water to obtain a mixed solution, pouring the mixed solution into a mold filled with a fiber mixture, and performing aging and drying treatment to obtain an aerogel thermal insulation material; wherein, calculated by volume ratio, the methyl triethoxysilane: distilled water: the absolute ethyl alcohol is 1 (2-3) to (2-3), ammonia water: the methyltriethoxysilane is 1 (20-30).
2. The preparation method of the high-efficiency aerogel thermal insulation material as claimed in claim 1, wherein the preparation method comprises the following steps:
in the step 2, the blended filter bag is cut into strips with the width of 5-10cm, and the strips are opened by a cloth opener to obtain a flocculent fiber mixture.
3. The preparation method of the high-efficiency aerogel thermal insulation material as claimed in claim 1, wherein the preparation method comprises the following steps:
in the step 3, the fiber mixture is soaked in oxalic acid solution with the mass fraction of 10-20% and sodium hypochlorite solution with the mass fraction of 5.5-10% for 12-24 h.
4. The preparation method of the high-efficiency aerogel thermal insulation material as claimed in claim 1, wherein the preparation method comprises the following steps:
in the step 4, the methyltriethoxysilane and the distilled water are mixed and stirred, and then the absolute ethyl alcohol and the ammonia water are poured for mixing and stirring.
5. The preparation method of the high-efficiency aerogel thermal insulation material as claimed in claim 1, wherein the preparation method comprises the following steps:
in the step 4, the molar concentration of the ammonia water is 10 mol/L.
6. The preparation method of the high-efficiency aerogel thermal insulation material as claimed in claim 1, wherein the preparation method comprises the following steps:
in the step 4, the aging temperature is 55-65 ℃, and the drying temperature is 80-100 ℃.
7. The method for preparing the high-efficiency aerogel thermal insulation material as claimed in claim 6, wherein the method comprises the following steps:
in the step 4, the aging time is 24-48h, and the drying time is 12-24 h.
8. The preparation method of the high-efficiency aerogel thermal insulation material as claimed in claim 1, wherein the preparation method comprises the following steps:
in the step 4, the filling rate of the fiber mixture in the aerogel thermal insulation material is 5-20%.
9. The preparation method of the high-efficiency aerogel thermal insulation material as claimed in claim 1, characterized in that:
in the step 4, the mixed solution is poured into a mould filled with the fiber mixture, then is kept stand for 30-60min, when the mixed solution is changed from colorless to turbid, absolute ethyl alcohol which is 2-4cm higher than the liquid level of the mould is poured into the mould, the mould is sealed for aging treatment, and after aging, the mould is opened, the mould is sealed and then is dried.
CN202210374240.2A 2022-04-11 2022-04-11 Preparation method of efficient aerogel heat-insulating material Active CN114804817B (en)

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Citations (6)

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Publication number Priority date Publication date Assignee Title
US20070259979A1 (en) * 2006-05-03 2007-11-08 Aspen Aerogels, Inc. Organic aerogels reinforced with inorganic aerogel fillers
CN103708476A (en) * 2014-01-07 2014-04-09 厦门大学 Preparation method of flexible silica aerogel
CN104629084A (en) * 2015-02-09 2015-05-20 浙江理工大学 Cleaning method of waste polytetrafluoroethylene filter bag
CN105666740A (en) * 2016-03-01 2016-06-15 浙江理工大学 Cleaning and recovering method for waste polytetrafluoroethylene and polyphenylene sulfide blended filter bag
CN109231953A (en) * 2018-10-31 2019-01-18 江苏华跃纺织新材料科技股份有限公司 The preparation method of high-performance fiber enhancing aerosil heat resistance filter bag material
CN109437829A (en) * 2018-10-31 2019-03-08 江苏华跃纺织新材料科技股份有限公司 The preparation method of broken invalid filter bag reclaiming fiber reinforcement base aeroge filter pocket material

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070259979A1 (en) * 2006-05-03 2007-11-08 Aspen Aerogels, Inc. Organic aerogels reinforced with inorganic aerogel fillers
CN103708476A (en) * 2014-01-07 2014-04-09 厦门大学 Preparation method of flexible silica aerogel
CN104629084A (en) * 2015-02-09 2015-05-20 浙江理工大学 Cleaning method of waste polytetrafluoroethylene filter bag
CN105666740A (en) * 2016-03-01 2016-06-15 浙江理工大学 Cleaning and recovering method for waste polytetrafluoroethylene and polyphenylene sulfide blended filter bag
CN109231953A (en) * 2018-10-31 2019-01-18 江苏华跃纺织新材料科技股份有限公司 The preparation method of high-performance fiber enhancing aerosil heat resistance filter bag material
CN109437829A (en) * 2018-10-31 2019-03-08 江苏华跃纺织新材料科技股份有限公司 The preparation method of broken invalid filter bag reclaiming fiber reinforcement base aeroge filter pocket material

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Title
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