CN111364239A - Silica aerogel heat preservation felt with long-acting conductivity and normal-pressure preparation method thereof - Google Patents

Silica aerogel heat preservation felt with long-acting conductivity and normal-pressure preparation method thereof Download PDF

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Publication number
CN111364239A
CN111364239A CN202010268638.9A CN202010268638A CN111364239A CN 111364239 A CN111364239 A CN 111364239A CN 202010268638 A CN202010268638 A CN 202010268638A CN 111364239 A CN111364239 A CN 111364239A
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material generated
ion exchange
conductivity
sodium silicate
silicon dioxide
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李仲亮
葛刚
胡毅
刘建
伍大海
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Tianjin Naco Century New Material Co ltd
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Tianjin Naco Century New Material Co ltd
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/77Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
    • D06M11/79Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/44Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic Table; Zincates; Cadmates
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/80Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with boron or compounds thereof, e.g. borides
    • D06M11/82Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with boron or compounds thereof, e.g. borides with boron oxides; with boric, meta- or perboric acids or their salts, e.g. with borax
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/285Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acid amides or imides

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Abstract

Discloses a method for preparing a silica aerogel heat preservation felt with long-acting conductivity under normal pressure, which comprises the following steps: 1. adding water into sodium silicate to prepare a silicon dioxide aqueous solution for later use; 2. adding cation exchange resin into an ion exchange column, and carrying out ion exchange on a sodium silicate aqueous solution through the ion exchange column; 3. adding the material generated in the step (2) into a dispersion grinding kettle, adjusting the pH value by using ammonia water, adding a stabilizer, adding an inorganic conductive agent, starting stirring, grinding and dispersing; 4. concentrating the material generated in the step (3), immersing the glass fiber mat into the solution at normal temperature, and fishing out after the glass fiber mat is saturated; 5. putting the material generated in the step (4) into a closed exchange tank, adding ammonia water, heating and preserving heat; 6. putting the material generated in the step 5 into a distillation kettle, adding n-butanol, heating to boil, and dehydrating and distilling; 7. and drying the mixture under the protection of nitrogen by utilizing microwave drying to prepare the silicon dioxide aerogel heat preservation felt with conductivity.

Description

Silica aerogel heat preservation felt with long-acting conductivity and normal-pressure preparation method thereof
Technical Field
The invention relates to the technical field of silicon dioxide aerogel, in particular to long-acting conductive silicon dioxide aerogel and a normal-pressure preparation method thereof.
Background
Silica-silica aerogel is known to be the lightest inorganic material found in the world today and having the best heat retaining property, and has excellent heat resistance as one of the functional materials, and thus has attracted attention as a next-generation heat insulating material.
However, since the silica aerogel is composed of fine particles of about 10nm, which are formed by point-to-point contact, the strength of the silica aerogel is poor. Therefore, in order to improve the strength, inorganic fibers and silica aerogel are compounded.
The high insulation of the silicon dioxide causes the phenomena that the silicon dioxide fiber felt is not easy to operate in the using process, the powder falls more and the powder is transferred to the surrounding environment. Due to the electrostatic effect, the silica aerogel also adsorbs dust impurities around the atmosphere, reducing the performance of the silica aerogel. In order to improve the antistatic property, some antistatic agents are needed to be added, but the action time is short, and the antistatic effect cannot be exerted for a long time.
Patent CN201611095569.6 discloses a method for producing silica aerogel, heat insulating material and silica aerogel, which uses sodium silicate and acid as raw materials to prepare sol, and then adds polymer conductive substance into the sol to form gel, so as to further prepare silica aerogel with conductivity. However, due to the addition of organic substances, the antistatic properties are affected by the volatilization of organic antistatic agents with the increase of the service time and at higher temperatures.
It can be seen that there is a need in the art for an improved solution for preparing silica aerogel insulation blankets having electrical conductivity.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a silicon dioxide aerogel heat preservation felt with long-acting conductivity and a normal-pressure preparation method thereof.
In one aspect of the invention, a method for preparing a silica aerogel insulation blanket with long-acting conductivity under normal pressure is provided, and the method comprises the following steps:
(1) preparing a sodium silicate aqueous solution;
(2) performing ion exchange on the sodium silicate aqueous solution and cation exchange resin;
(3) adding the material generated in the step (2) into a dispersion grinding kettle, adjusting the pH value with ammonia water, adding a stabilizer, adding an inorganic conductive agent, and stirring to grind and disperse;
(4) after concentrating the material generated in the step (3), immersing the glass fiber felt into the solution, and fishing out after the glass fiber felt is saturated;
(5) putting the material generated in the step (4) into a closed exchange tank, adding ammonia water, heating and preserving heat;
(6) putting the material generated in the step (5) into a distillation kettle, adding n-butanol, heating to boil, and performing dehydration distillation; and
(7) and drying the mixture under the protection of nitrogen by utilizing microwave drying to prepare the silicon dioxide aerogel heat preservation felt with conductivity.
In another aspect of the invention, there is provided a silica aerogel insulation blanket having long-term conductivity prepared using an atmospheric preparation method of a silica aerogel insulation blanket having long-term conductivity according to any one of the embodiments of the invention.
The silica aerogel heat preservation felt with long-acting conductivity prepared by the method disclosed by the embodiment of the invention overcomes the defects of the prior art due to the use of the inorganic conductive agent, and still has better antistatic performance at the temperature of 200-400 ℃. In addition, by adding the stabilizer, the aerogel structure is stabilized, and the performance and the service life of the silica aerogel heat-insulating felt are further improved.
Drawings
FIG. 1 shows a flow diagram of an atmospheric pressure method for making an aerogel insulation blanket having long-lasting conductivity in accordance with an embodiment of the present invention.
Detailed Description
Embodiments of the present invention are described in detail below with reference to the accompanying drawings. In the following description, numerous specific details are set forth in order to provide a more thorough understanding of the present invention to those skilled in the art. It will be apparent, however, to one skilled in the art that the present invention may be practiced without some of these specific details. Furthermore, it should be understood that the invention is not limited to the specific embodiments described. Rather, it is contemplated that the invention may be practiced with any combination of the following features and elements, whether or not they relate to different embodiments. Thus, the following aspects, features, embodiments and advantages are merely illustrative and should not be considered elements or limitations of the claims except where explicitly recited in a claim. The meaning of each term referred to in this specification is generally a meaning commonly understood in the art or a meaning normally understood by those skilled in the art after reading this specification. The terms "comprising" and "including" in this specification are open-ended, i.e., may include additional elements not already mentioned in addition to the elements already mentioned. The specific values of the contents of the components described in the present specification are only used to indicate a proportional relationship between the contents of the components, and are not used to limit the contents of the components to any absolute values. Specific values for the amounts of ingredients and specific values for process conditions described in this specification are intended to be inclusive of one another, e.g., 15% inclusive, and are not intended to be limiting to a precise value.
FIG. 1 illustrates an atmospheric pressure method for preparing a silica aerogel insulation blanket having long-lasting conductivity according to an embodiment of the present invention. As shown in fig. 1, the method comprises the steps of:
(1) preparing a sodium silicate aqueous solution;
(2) performing ion exchange on the sodium silicate aqueous solution and cation exchange resin;
(3) adding the material generated in the step (2) into a dispersion grinding kettle, adjusting the pH value with ammonia water, adding a stabilizer, adding an inorganic conductive agent, and stirring to grind and disperse;
(4) after concentrating the material generated in the step (3), immersing the glass fiber felt into the solution, and fishing out after the glass fiber felt is saturated;
(5) putting the material generated in the step (4) into a closed exchange tank, adding ammonia water, heating and preserving heat;
(6) putting the material generated in the step (5) into a distillation kettle, adding n-butanol, heating to boil, and performing dehydration distillation; and
(7) and drying the mixture under the protection of nitrogen by utilizing microwave drying to prepare the silicon dioxide aerogel heat preservation felt with conductivity.
In some embodiments, in said step (1), the sodium silicate is added with water to prepare an aqueous solution of 5 to 10wt% based on silica.
In some embodiments, in step (2), the cation exchange resin is added to the ion exchange column, the aqueous sodium silicate solution produced in step (1) is subjected to ion exchange through the ion exchange column, and the outlet PH3-4 of the ion exchange column is adjusted.
In some embodiments, in the step (3), the material generated in the step (2) is added into a dispersion grinding kettle, the pH is adjusted to 6-8 by ammonia water, a stabilizer accounting for 1-3% of silicon dioxide is added, and the mixture is stirred for 20-30 minutes; adding inorganic conductive agent with the dosage of 5-10wt% of the silicon dioxide, starting stirring, and grinding and dispersing for 30-40 minutes at 1500-2000 r/min.
In some embodiments, in step (3), the stabilizing agent is selected from one or more of polyacrylamide and derivatives.
In some embodiments, in the step (3), the inorganic conductive agent is selected from one or more of zirconium diborate, titanium diborate and nano zinc oxide.
In some embodiments, in the step (4), the material generated in the step (3) is concentrated to a silica content of 10-20 wt%, and the glass fiber mat is immersed into the solution at normal temperature and taken out until saturated.
In some embodiments, in the step (5), the material generated in the step (4) is placed in a closed exchange tank, ammonia water is added, the temperature is increased to 80-90 ℃, the pH value of 8-9 in the tank is maintained, and the temperature is maintained for 1-2 hours.
In some embodiments, in the step (6), the material generated in the step (5) is placed in a distillation kettle, n-butanol is added, the temperature is increased to boiling for dehydration distillation, and the distillation is stopped when the distillation temperature reaches 110-.
In some embodiments, in the step (7), microwave drying is performed under the protection of nitrogen, wherein the drying temperature is 110-.
The method for preparing the silica aerogel insulation blanket with long-acting conductivity under normal pressure according to the embodiment of the invention is described above with reference to the attached drawings, and it should be noted that the above description is only an example and not a limitation of the invention. In other embodiments of the invention, the method may include more, fewer, or different process steps, and the ingredients, proportions, and process conditions and parameters in the various process steps may differ from those described and illustrated.
In another aspect of the invention, there is also provided a silica aerogel insulation blanket with long-term conductivity prepared using an atmospheric preparation method of a silica aerogel insulation blanket with long-term conductivity according to any one of the embodiments of the invention.
Several specific embodiments of the invention are described below:
example one
1. Adding water into sodium silicate to prepare 1000g of water solution with the weight percent of 5 percent calculated by silicon dioxide for standby;
2. adding cation exchange resin into an ion exchange column, performing ion exchange on the sodium silicate generated in the step (1) through the ion exchange column, and adjusting the pH value of an outlet of the ion exchange column to be 4.0;
3. adding the material generated in the step 2 into a dispersion grinding kettle, adjusting the pH value to 6.0 by using ammonia water, adding 0.5g of anionic polyacrylamide and 2.5g of zirconium diborate inorganic conductive agent, starting stirring, and grinding and dispersing for 40 minutes at 1500 r/min;
4. concentrating the material generated in the step (3) until the content of silicon dioxide is 10wt%, soaking the glass fiber mat into the solution at normal temperature until the glass fiber mat is saturated, and fishing out;
5. putting the material generated in the step 4 into a closed exchange tank, adding ammonia water, heating to 80 ℃, keeping the pH9 in the tank, and keeping the temperature for 2 hours;
6. putting the material generated in the step 5 into a distillation kettle, adding n-butanol, heating to boil for dehydrating and distilling, and stopping distilling when the distillation temperature reaches 115 ℃;
7. and drying the mixture at the temperature of 110 ℃ for 4 hours by using a microwave dryer under the protection of nitrogen, thereby preparing the conductive silicon dioxide aerogel heat preservation felt.
Example two
1. Adding water into sodium silicate to prepare 1000g of water solution with the weight percent of 8 percent of silicon dioxide for standby;
2. adding cation exchange resin into an ion exchange column, performing ion exchange on sodium silicate through the ion exchange column, and adjusting the pH value of an outlet of the ion exchange column to be 3.0;
3. adding the material generated in the step 2 into a dispersion grinding kettle, adjusting the pH value to 6.5 by using ammonia water, adding 1.6g of nonionic polyacrylamide and 5g of titanium diborate inorganic conductive agent, starting stirring, and grinding and dispersing for 40 minutes at 1500 r/min;
4. concentrating the material generated in the step (3) until the content of silicon dioxide is 12wt%, soaking the glass fiber mat into the solution at normal temperature until the glass fiber mat is saturated, and fishing out;
5. putting the material generated in the step 4 into a closed exchange tank, adding ammonia water, heating to 80 ℃, keeping the pH of 9 in the tank, and preserving the heat for 1.5 hours;
6. putting the material generated in the step 5 into a distillation kettle, adding n-butanol, heating to boil for dehydrating and distilling, and stopping distilling when the distillation temperature reaches 112 ℃;
7. and drying the mixture by using a microwave dryer under the protection of nitrogen at the drying temperature of 110 ℃ for 4.5 hours to prepare the conductive silicon dioxide aerogel heat-preservation felt.
EXAMPLE III
1. Adding water into sodium silicate to prepare 1000g of 10wt% aqueous solution calculated by silicon dioxide for later use;
2. adding cation exchange resin into an ion exchange column, performing ion exchange on sodium silicate through the ion exchange column, and adjusting the pH value of an outlet of the ion exchange column to be 3.0;
3. adding the material generated in the step 2 into a dispersion grinding kettle, adjusting the pH value to 8.0 by using ammonia water, adding 10g of cationic polyacrylamide and 10g of nano zinc oxide inorganic conductive agent, starting stirring, and grinding and dispersing for 40 minutes at 2000 r/min;
4. concentrating the material generated in the step (3) until the content of silicon dioxide is 15wt%, soaking the glass fiber mat into the solution at normal temperature until the glass fiber mat is saturated, and fishing out;
5. putting the material generated in the step 4 into a closed exchange tank, adding ammonia water, heating to 90 ℃, keeping the pH9 in the tank, and keeping the temperature for 1 hour;
6. putting the material generated in the step 5 into a distillation kettle, adding n-butanol, heating to boil for dehydrating and distilling, and stopping distilling when the distillation temperature reaches 110 ℃;
7. and drying the mixture at the temperature of 110 ℃ for 5 hours by using a microwave dryer under the protection of nitrogen, thereby preparing the conductive silicon dioxide aerogel heat preservation felt.
Performance testing
Conductive agent Resistance order of magnitude (omega) (120 deg.C)
Example one Zirconium diborate 10x109
Example two Titanium diborate 10x109
EXAMPLE III Nano zinc oxide 10x109
Comparative example Is free of 10x1012
The silica aerogel heat preservation felt with long-acting conductivity prepared by the method disclosed by the embodiment of the invention overcomes the defects of the prior art due to the use of the inorganic conductive agent, and still has better antistatic performance at the temperature of 200-400 ℃. In addition, by adding the stabilizer, the aerogel structure is stabilized, and the performance and the service life of the silica aerogel heat-insulating felt are further improved.
Although the present invention has been disclosed above by way of examples, the present invention is not limited thereto. Various changes and modifications within the spirit and scope of the invention will become apparent to those skilled in the art from this disclosure, and the scope of the invention should be determined only by the language of the claims and the equivalents thereof.

Claims (10)

1. A method for preparing a silica aerogel heat preservation felt with long-acting conductivity under normal pressure comprises the following steps:
(1) preparing a sodium silicate aqueous solution;
(2) performing ion exchange on the sodium silicate aqueous solution and cation exchange resin;
(3) adding the material generated in the step (2) into a dispersion grinding kettle, adjusting the pH value with ammonia water, adding a stabilizer, adding an inorganic conductive agent, and stirring to grind and disperse;
(4) after concentrating the material generated in the step (3), immersing the glass fiber felt into the solution, and fishing out after the glass fiber felt is saturated;
(5) putting the material generated in the step (4) into a closed exchange tank, adding ammonia water, heating and preserving heat;
(6) putting the material generated in the step (5) into a distillation kettle, adding n-butanol, heating to boil, and performing dehydration distillation; and
(7) and drying the mixture under the protection of nitrogen by utilizing microwave drying to prepare the silicon dioxide aerogel heat preservation felt with conductivity.
2. The method as claimed in claim 1, wherein, in the step (1), the sodium silicate is added with water to prepare an aqueous solution of 5-10wt% in terms of silica.
3. The method according to claim 1, wherein in the step (2), cation exchange resin is added into the ion exchange column, the aqueous sodium silicate solution generated in the step (1) is subjected to ion exchange through the ion exchange column, and the outlet pH3-4 of the ion exchange column is adjusted.
4. The method as claimed in claim 1, wherein, in the step (3), the material generated in the step (2) is added into a dispersion grinding kettle, the pH is adjusted to 6-8 by ammonia water, a stabilizer accounting for 1-3% of the silicon dioxide is added, and the mixture is stirred for 20-30 minutes; adding inorganic conductive agent with the dosage of 5-10wt% of the silicon dioxide, starting stirring, and grinding and dispersing for 30-40 minutes at 1500-2000 r/min.
5. The method according to claim 1, wherein in the step (4), the material produced in the step (3) is concentrated to a silica content of 10-20 wt%, and the glass fiber mat is immersed into the solution at normal temperature, taken out until saturated.
6. The method according to claim 1, wherein in the step (5), the material generated in the step (4) is placed in a closed exchange tank, ammonia water is added, the temperature is raised to 80-90 ℃, the pH value in the tank is kept at 8-9, and the temperature is kept for 1-2 hours.
7. The method as claimed in claim 1, wherein in the step (7), the silica aerogel thermal insulation felt with conductivity is prepared by drying with microwave under the protection of nitrogen at the drying temperature of 110 ℃ and 120 ℃ for 4-5 hours.
8. The method according to claim 1, wherein, in the step (3), the stabilizer is selected from one or more of polyacrylamide and derivatives.
9. The method according to claim 1, wherein in the step (3), the inorganic conductive agent is selected from one or more of zirconium diborate, titanium diborate and nano zinc oxide.
10. A silica aerogel insulation blanket having long lasting conductivity prepared using the method of any of claims 1-9.
CN202010268638.9A 2020-04-08 2020-04-08 Silica aerogel heat preservation felt with long-acting conductivity and normal-pressure preparation method thereof Pending CN111364239A (en)

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