Preparation method of aluminum silicate fiber-reinforced aerogel felt and impregnation reactor

Abstract

The present disclosure provides a preparation method of an aluminum silicate fiber-reinforced aerogel felt, including the following steps: mixing orthosilicate, ethanol, and water evenly, adding an NH.sub.4F solution and ammonia water successively, and stirring evenly to obtain a silica sol; winding an aluminum silicate fiber felt into a roll and mounting on a rotatable central shaft of a impregnation reaction kettle; where a plurality of injection holes are equidistantly provided on a surface of the reaction kettle; the central shaft of the reaction kettle drives the aluminum silicate fiber felt to rotate and slowly inject the silica sol into the surface of the fiber felt through the injection holes to conduct the impregnation; allowing the fiber felt-gel composite to stand to conduct aging; placing the aged fiber felt-gel composite in absolute ethanol to conduct solvent replacement to remove moisture; and drying to obtain the aluminum silicate fiber-reinforced aerogel felt.

Claims

1. A preparation method of an aluminum silicate fiber-reinforced aerogel felt, comprising: (1) mixing orthosilicate, ethanol, and water evenly, adding an NH4F solution and ammonia water successively, and stirring evenly to obtain a silica sol; wherein the orthosilicate, the ethanol, and water have a molar ratio of 1:(4-12):(2-4); the NH.sub.4F solution is added with a molar ratio of NH.sub.4F and the orthosilicate at (0.002-0.01):1; and the ammonia water is added with a molar ratio of NH.sub.3 and the orthosilicate at (0.005-0.015):1; (2) winding an aluminum silicate fiber felt into a roll and mounting on a rotatable central shaft of a reaction kettle; wherein the central shaft is parallel to the ground and rotatable, and a plurality of injection holes are provided on a surface of the reaction kettle; rotating the central shaft to drive the aluminum silicate fiber felt to rotate, and injecting the silica sol into the reaction kettle through the plurality of injection holes to impregnate the aluminum silicate fiber felt, a fiber felt-gel composite being obtained after the aluminum silicate fiber felt being impregnated; (3) making the fiber felt-gel composite obtained in (2) to stand to conduct aging at 30 C. to 60 C. for 8 h to 24 h; (4) placing the fiber felt-gel composite obtained in (3) in absolute ethanol to conduct solvent replacement multiple times to remove excess water in the fiber felt-gel composite; and (5) drying the fiber felt-gel composite obtained in (4) to obtain the aluminum silicate fiber-reinforced aerogel felt.

2. The preparation method of an aluminum silicate fiber-reinforced aerogel felt according to claim 1, wherein in (1), the orthosilicate is one selected from the group consisting of tetraethyl orthosilicate (TEOS), tetramethyl orthosilicate (TMOS), and tetraisopropyl orthosilicate (TIPOS).

3. The preparation method of an aluminum silicate fiber-reinforced aerogel felt according to claim 1, wherein in (2), the impregnation is conducted for 12 h to 24 h.

4. The preparation method of an aluminum silicate fiber-reinforced aerogel felt according to claim 1, wherein in (4), the solvent replacement is conducted 2 to 3 times with 12 h to 36 h in each time.

5. The preparation method of an aluminum silicate fiber-reinforced aerogel felt according to claim 1, wherein the reaction kettle comprises a body of the reaction kettle and the central shaft in the body of the reaction kettle, the plurality of injection holes are equidistantly provided on a surface of the body of the reaction kettle; and an aluminum silicate fiber felt roll is wound on the central shaft of the reaction kettle.

6. The preparation method of an aluminum silicate fiber-reinforced aerogel felt according to claim 5, wherein the body of the reaction kettle has an inner diameter 1.2 to 1.5 times an outer diameter of the aluminum silicate fiber felt roll.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

(1) FIG. 1 shows a structural schematic diagram of an impregnation reactor in the present disclosure;

(2) FIG. 2 shows a top view of FIG. 1; and

(3) FIG. 3 shows a plane view of FIG. 1 along a direction of a central shaft; where

(4) in the figure: 1 is a central shaft, 2 is a reactor body, 3 is an injection hole, and 4 is a fiber felt roll.

DETAILED DESCRIPTION OF THE EMBODIMENTS

(5) The present disclosure will be further described below in conjunction with specific examples and the accompanying drawings. It should be understood that these examples are only intended to describe the present disclosure, rather than to limit the scope of the present disclosure.

EXAMPLE 1

(6) A preparation method of an aluminum silicate fiber-reinforced aerogel felt included the following steps: (1) TEOS, ethanol, and water were mixed evenly, an NH.sub.4F solution and ammonia water were added successively, and stirred evenly to obtain a silica sol; where the TEOS, the ethanol, and water had a molar ratio of 1:5:2; the NH.sub.4F solution was added with a molar ratio of NH.sub.4F and the TEOS at 0.003:1; and the ammonia water was added with a molar ratio of NH.sub.3 and the TEOS at 0.006:1; (2) an aluminum silicate fiber felt was wound into a roll and mounted on a rotatable central shaft of a impregnation reactor; where the central shaft was parallel to the ground and rotatable, and a plurality of injection holes were equidistantly provided on a surface of the during impregnation, the central shaft of the reactor drove the aluminum silicate fiber felt to rotate and slowly inject the silica sol obtained in step (1) is slowly injected into the surface of the fiber felt through the injection holes to conduct the impregnation; (3) the fiber felt-gel composite obtained after being subjected to the impregnation in step (2) was allowed to stand to conduct aging at 30 C. for 20 h; (4) the fiber felt-gel composite obtained in step (3) was placed in absolute ethanol to conduct solvent replacement multiple times to remove excess water in the fiber felt-gel composite; and (5) the fiber felt-gel composite obtained in step (4) was dried to obtain the aluminum silicate fiber-reinforced aerogel felt.

(7) In step (2), the impregnation was conducted for 15 h.

(8) In step (4), the solvent replacement was conducted 2 times with 16 h in each time.

(9) In step (2), referring to FIG. 1, FIG. 2, and FIG. 3, the impregnation reactor included a reactor central shaft (1) and a reactor body (2), where a plurality of the injection holes (3) were equidistantly provided on a surface of the reactor body (2); and an aluminum silicate fiber felt roll (4) was wound on the reactor central shaft (1); and the reactor body (2) had an inner diameter 1.2 times an outer diameter of the aluminum silicate fiber felt roll (4).

EXAMPLE 2

(10) A preparation method of an aluminum silicate fiber-reinforced aerogel felt included the following steps: (1) TMOS, ethanol, and water were mixed evenly, an NH.sub.4F solution and ammonia water were added successively, and stirred evenly to obtain a silica sol; where the TMOS, the ethanol, and water had a molar ratio of 1:5:2; the NH.sub.4F solution was added with a molar ratio of NH.sub.4F and the TMOS at 0.005:1; and the ammonia water was added with a molar ratio of NH.sub.3 and the TMOS at 0.008:1; (2) an aluminum silicate fiber felt was wound into a roll and mounted on a rotatable central shaft of a impregnation reactor; where the central shaft was parallel to the ground and rotatable, and a plurality of injection holes were equidistantly provided on a surface of the reactor; during impregnation, the central shaft of the reactor drove the aluminum silicate fiber felt to rotate and slowly inject the silica sol obtained in step (1) is slowly injected into the surface of the fiber felt through the injection holes to conduct the impregnation; (3) the fiber felt-gel composite obtained after being subjected to the impregnation in step (2) was allowed to stand to conduct aging at 40 C. for 22 h; (4) the fiber felt-gel composite obtained in step (3) was placed in absolute ethanol to conduct solvent replacement multiple times to remove excess water in the fiber felt-gel composite; and (5) the fiber felt-gel composite obtained in step (4) was dried to obtain the aluminum silicate fiber-reinforced aerogel felt.

(11) In step (2), the impregnation was conducted for 18 h.

(12) In step (4), the solvent replacement was conducted 3 times with 15 h in each time.

(13) In step (2), referring to FIG. 1, FIG. 2, and FIG. 3, the impregnation reactor included a reactor central shaft (1) and a reactor body (2), where a plurality of the injection holes (3) were equidistantly provided on a surface of the reactor body (2); and an aluminum silicate fiber felt roll (4) was wound on the reactor central shaft (1); and the reactor body (2) had an inner diameter 1.3 times an outer diameter of the aluminum silicate fiber felt roll (4).

EXAMPLE 3

(14) A preparation method of an aluminum silicate fiber-reinforced aerogel felt included the following steps: (1) TIPOS, ethanol, and water were mixed evenly, an NH.sub.4F solution and ammonia water were added successively, and stirred evenly to obtain a silica sol; where the TIPOS, the ethanol, and water had a molar ratio of 1:8:4; the NH.sub.4F solution was added with a molar ratio of NH.sub.4F and the TIPOS at 0.006:1; and the ammonia water was added with a molar ratio of NH.sub.3 and the TIPOS at 0.009:1; (2) an aluminum silicate fiber felt was wound into a roll and mounted on a rotatable central shaft of a impregnation reactor; where, the central shaft was parallel to the ground and rotatable, and a plurality of injection holes were equidistantly provided on a surface of the reactor; during impregnation, the central shaft of the reactor drove the aluminum silicate fiber felt to rotate and slowly inject the silica sol obtained in step (1) is slowly injected into the surface of the fiber felt through the injection holes to conduct the impregnation; (3) the fiber felt-gel composite obtained after being subjected to the impregnation in step (2) was allowed to stand to conduct aging at 50 C. for 12 h; (4) the fiber felt-gel composite obtained in step (3) was placed in absolute ethanol to conduct solvent replacement multiple times to remove excess water in the fiber felt-gel composite; and (5) the fiber felt-gel composite obtained in step (4) was dried to obtain the aluminum silicate fiber-reinforced aerogel felt.

(15) In step (2), the impregnation was conducted for 20 h.

(16) In step (4), the solvent replacement was conducted 2 times with 19 h in each time.

(17) In step (2), referring to FIG. 1, FIG. 2, and FIG. 3, the impregnation reactor included a reactor central shaft (1) and a reactor body (2), where a plurality of the injection holes (3) were equidistantly provided on a surface of the reactor body (2); and an aluminum silicate fiber felt roll (4) was wound on the reactor central shaft (1); and the reactor body (2) had an inner diameter 1.4 times an outer diameter of the aluminum silicate fiber felt roll (4).

EXAMPLE 4

(18) A preparation method of an aluminum silicate fiber-reinforced aerogel felt included the following steps: (1) TMOS, ethanol, and water were mixed evenly, an NH.sub.4F solution and ammonia water were added successively, and stirred evenly to obtain a silica sol; where the TMOS, the ethanol, and water had a molar ratio of 1:9:3; the NH.sub.4F solution was added with a molar ratio of NH.sub.4F and the TMOS at 0.008:1; and the ammonia water was added with a molar ratio of NH.sub.3 and the TMOS at 0.012:1; (2) an aluminum silicate fiber felt was wound into a roll and mounted on a rotatable central shaft of a impregnation reactor; where the central shaft was parallel to the ground and rotatable, and a plurality of injection holes were equidistantly provided on a surface of the reactor; during impregnation, the central shaft of the reactor drove the aluminum silicate fiber felt to rotate and slowly inject the silica sol obtained in step (1) is slowly injected into the surface of the fiber felt through the injection holes to conduct the impregnation; (3) the fiber felt-gel composite obtained after being subjected to the impregnation in step (2) was allowed to stand to conduct aging at 55 C. for 8 h; (4) the fiber felt-gel composite obtained in step (3) was placed in absolute ethanol to conduct solvent replacement multiple times to remove excess water in the fiber felt-gel composite; and (5) the fiber felt-gel composite obtained in step (4) was dried to obtain the aluminum silicate fiber-reinforced aerogel felt.

(19) In step (2), the impregnation was conducted for 21 h.

(20) In step (4), the solvent replacement was conducted 3 times with 32 h in each time.

(21) In step (2), referring to FIG. 1, FIG. 2, and FIG. 3, the impregnation reactor included a reactor central shaft (1) and a reactor body (2), where a plurality of the injection holes (3) were equidistantly provided on a surface of the reactor body (2); and an aluminum silicate fiber felt roll (4) was wound on the reactor central shaft (1); and the reactor body (2) had an inner diameter 1.5 times an outer diameter of the aluminum silicate fiber felt roll (4).

EXAMPLE 5

(22) A preparation method of an aluminum silicate fiber-reinforced aerogel felt included the following steps: (1) TEOS, ethanol, and water were mixed evenly, an NH.sub.4F solution and ammonia water were added successively, and stirred evenly to obtain a silica sol; where the TEOS, the ethanol, and water had a molar ratio of 1:7:3; the NH.sub.4F solution was added with a molar ratio of NH.sub.4F and the TEOS at 0.007:1; and the ammonia water was added with a molar ratio of NH.sub.3 and the TEOS at 0.013:1; (2) an aluminum silicate fiber felt was wound into a roll and mounted on a rotatable central shaft of a impregnation reactor; where the central shaft was parallel to the ground and rotatable, and a plurality of injection holes were equidistantly provided on a surface of the reactor; during impregnation, the central shaft of the reactor drove the aluminum silicate fiber felt to rotate and slowly inject the silica sol obtained in step (1) is slowly injected into the surface of the fiber felt through the injection holes to conduct the impregnation; (3) the fiber felt-gel composite obtained after being subjected to the impregnation in step (2) was allowed to stand to conduct aging at 60 C. for 15 h; (4) the fiber felt-gel composite obtained in step (3) was placed in absolute ethanol to conduct solvent replacement multiple times to remove excess water in the fiber felt-gel composite; and (5) the fiber felt-gel composite obtained in step (4) was dried to obtain the aluminum silicate fiber-reinforced aerogel felt.

(23) In step (2), the impregnation was conducted for 15 h.

(24) In step (4), the solvent replacement was conducted 2 times with 25 h in each time.

(25) In step (2), referring to FIG. 1, FIG. 2, and FIG. 3, the impregnation reactor included a reactor central shaft (1) and a reactor body (2), where a plurality of the injection holes (3) were equidistantly provided on a surface of the reactor body (2); and an aluminum silicate fiber felt roll (4) was wound on the reactor central shaft (1); and the reactor body (2) had an inner diameter 1.3 times an outer diameter of the aluminum silicate fiber felt roll (4).

EXAMPLE 6

(26) A preparation method of an aluminum silicate fiber-reinforced aerogel felt included the following steps: (1) TIPOS, ethanol, and water were mixed evenly, an NH.sub.4F solution and ammonia water were added successively, and stirred evenly to obtain a silica sol; where the TIPOS, the ethanol, and water had a molar ratio of 1:10:4; the NH.sub.4F solution was added with a molar ratio of NH.sub.4F and the TIPOS at 0.009:1; and the ammonia water was added with a molar ratio of NH.sub.3 and the TWOS at 0.007:1; (2) an aluminum silicate fiber felt was wound into a roll and mounted on a rotatable central shaft of a rotatable impregnation reactor; where the central shaft was parallel to the ground and rotatable, and a plurality of injection holes were equidistantly provided on a surface of the reactor; during impregnation, the central shaft of the reactor drove the aluminum silicate fiber felt to rotate and slowly inject the silica sol obtained in step (1) is slowly injected into the surface of the fiber felt through the injection holes to conduct the impregnation; (3) the fiber felt-gel composite obtained after being subjected to the impregnation in step (2) was allowed to stand to conduct aging at 50 C. for 20 h; (4) the fiber felt-gel composite obtained in step (3) was placed in absolute ethanol to conduct solvent replacement multiple times to remove excess water in the fiber felt-gel composite; and (5) the fiber felt-gel composite obtained in step (4) was dried to obtain the aluminum silicate fiber-reinforced aerogel felt.

(27) In step (2), the impregnation was conducted for 20 h.

(28) In step (4), the solvent replacement was conducted 2 times with 20 h in each time.

(29) In step (2), referring to FIG. 1, FIG. 2, and FIG. 3, the impregnation reactor included a reactor central shaft (1) and a reactor body (2), where a plurality of the injection holes (3) were equidistantly provided on a surface of the reactor body (2); and an aluminum silicate fiber felt roll (4) was wound on the reactor central shaft (1); and the reactor body (2) had an inner diameter 1.4 times an outer diameter of the aluminum silicate fiber felt roll (4).

(30) The above examples are merely preferred examples of the present disclosure and are not intended to limit the present disclosure, and various changes and modifications may be made to the present disclosure by those skilled in the art. Any modification, equivalent substitution, improvement and the like made within the spirit and principle of the present disclosure shall fall within the protection scope of the present disclosure.