CN111962296A

CN111962296A - Aerogel textile fabric and preparation method thereof

Info

Publication number: CN111962296A
Application number: CN202010780649.5A
Authority: CN
Inventors: 王金富; 韩进亮; 丁建涛; 李姝华
Original assignee: Individual
Current assignee: Individual
Priority date: 2020-08-06
Filing date: 2020-08-06
Publication date: 2020-11-20

Abstract

The invention discloses an aerogel textile fabric and a preparation method thereof, wherein the preparation method comprises the following steps: s1, adding the precursor into a reaction kettle, adding a catalyst, and uniformly stirring to obtain sol with rheological property; s2, spraying the obtained sol on DTY (draw textured yarn), standing to obtain wet gel, and obtaining DTY (draw textured yarn) loaded with wet gel; s3, sequentially carrying out solvent replacement, hydrophobic reaction and drying on the wet gel-loaded DTY (draw textured yarn) to obtain aerogel modified DTY (draw textured yarn); s4, weaving with aerogel modified DTY (draw textured yarn) to obtain the aerogel textile fabric. The invention has the advantages of good warm-keeping effect, light and thin texture and wide application range.

Description

Aerogel textile fabric and preparation method thereof

Technical Field

The invention relates to the technical field of textile fabrics, in particular to an aerogel textile fabric and a preparation method thereof.

Background

Partial items of modern ice and snow sports are devoured from military operations, and like cold protective clothing guarantees the life safety of soldiers, the cold protective clothing is also a particularly important factor influencing the physical health of athletes and the game performance. Therefore, the research on the warm-keeping fabric for making the cold protective clothing is more and more concerned by people.

The invention patent application with application publication number CN108773125A discloses a thermal fabric, which comprises three layers of fabrics, wherein the inner layer is a thermal layer, the surface layer is a windproof layer, the middle layer is a wear-resistant layer, the three layers are connected by sewing cotton threads, the inner layer is a full-cotton fabric, the fabrics are provided with a plurality of concave-convex structures, the concave-convex structures are covered with cow hair fiber and sheep wool fiber, and the number of the concave-convex structures is 10.

In view of the above-mentioned related arts, the inventors believe that the number of layers of the fabric is large, and the fabric is warm for producing the sportswear, but has a problem of heavy weight, and the heavy weight of the sportswear affects the technical performance due to the fact that the ice and snow project is blended with both the speed and the great amount of the sport skills, so that the fabric produced by the above-mentioned related arts is difficult to meet the market demand of the sportswear.

Disclosure of Invention

Aiming at the defects in the prior art, the first purpose of the invention is to provide an aerogel textile fabric which has the advantages of good warm-keeping effect, light and thin texture and wide application range.

In order to achieve the first object, the invention provides the following technical scheme: a preparation method of an aerogel textile fabric comprises the following steps:

s1, adding the precursor into a reaction kettle, adding a catalyst, and uniformly stirring to obtain sol with rheological property;

s2, spraying the obtained sol on DTY (draw textured yarn), standing to obtain wet gel, and obtaining DTY (draw textured yarn) loaded with wet gel;

s3, sequentially carrying out solvent replacement, hydrophobic reaction and drying on the wet gel-loaded DTY (draw textured yarn) to obtain aerogel modified DTY (draw textured yarn);

s4, weaving with aerogel modified DTY (draw textured yarn) to obtain the aerogel textile fabric.

Through adopting above-mentioned technical scheme, combine together the thermal-insulated heat preservation characteristic of aerogel and DTY (tensile deformation silk) can weave the characteristic, form the aerogel textile fabric that has each item characteristic of aerogel, its thermal conductivity is less than still air, and thermal insulation performance is far beyond ordinary fibre. Meanwhile, the fabric woven by the same weaving process of the same thick and thin yarns is 18% -21% lighter than the fabric made by common yarns, but the heat-insulating property of the made single-piece garment is improved by 20-40% different from that of the common material.

In addition, based on the characteristic of high specific surface area of the aerogel, the aerogel textile fabric also has the characteristics of quick drying, peculiar smell resistance, easiness in dyeing and low static electricity.

Further, in the s3 step, the solvent replacement uses ethanol to replace water in the sol.

By adopting the technical scheme, the water in the sol is replaced by the ethanol, so that the liquid interfacial tension of the gel framework is reduced, the Si-OH on the surfaces of the pore channels of the sol is modified by the ethanol, the reaction between the Si-OH and water molecules in the air is prevented, the loss of the pore structure of the aerogel can be reduced, and the weight of the aerogel textile fabric is reduced and the heat retention property is enhanced.

Further, in the step s3, the hydrophobic reaction is hydrophobically modified by methyl trimethylsilane, vinyl trimethylsilane and phenyl trimethoxysilane, wherein the weight ratio of methyl trimethylsilane, vinyl trimethylsilane and phenyl trimethoxysilane is 3: (1-4): (8-11).

By adopting the technical scheme, the gel framework is subjected to hydrophobic modification through compounding of methyl trimethylsilane, vinyl trimethylsilane and phenyl trimethoxy silane, so that the pressure condition for drying the gel framework can be reduced, the damage of water vapor in the air to the gel framework is reduced, the heat retention of the aerogel textile fabric is improved, the process difficulty can be reduced, and the production is facilitated.

Further, in the step s1, the precursor includes polyamide and tetraethoxysilane, and the weight ratio of the polyamide to tetraethoxysilane is (2-5): 13.

by adopting the technical scheme, the composite sol obtained by the reaction of the polyamide and the tetraethoxysilane in the reaction kettle is complementary by utilizing the advantages of the polyamide and the tetraethoxysilane, so that the aperture of the aerosol can be reduced, and the aerosol is more smooth and skin-friendly, can reduce irritation and friction to the skin, and is more comfortable to use.

Further, in the step s1, the pH is adjusted to 4-6.

By adopting the technical scheme, the polyethylene glycol and the tetraethoxysilane are subjected to step-by-step degressive fractional hydrolysis reaction at first, the hydrolysis products are mutually condensed to generate sol, the condensation reaction is slowed down under the acidic condition, the gelation time is prolonged, the sol particles are cross-linked and loose, and the three-dimensional molecular network sol is finally formed, so that the flexibility and the folding resistance of the aerogel textile fabric are improved, the service life of the aerogel textile fabric is prolonged, the sports wear attached to a human body can be further manufactured, the application and exhibition actions are facilitated, and the clothes are light, warm and have a wide application range.

Further, in the step s3, CO is used for drying₂As a medium.

By adopting the technical scheme, the CO₂The critical temperature is low, the aerogel is non-toxic and can not be combusted, the recycling can be realized, the resources are saved, the use is safe, and the purity of the prepared aerogel is high.

Further, in the s2 step, the preparation method of DTY (draw textured yarn) comprises the following steps:

s1, adding petroleum base, plant base and polyester fiber into a reaction kettle for reaction to obtain polymer melt;

s2, cooling and solidifying the polymer melt, and cutting to obtain granules;

s3, drying the cut particles until the water content is less than 25ppm, performing melt spinning to prepare POY (pre-oriented yarn taking), and then performing drawing and twisting to prepare DTY (draw textured yarn).

By adopting the technical scheme, the softening point of the polyester can be improved when the polyester is dried until the water content is less than 25ppm, the ring knot blocking phenomenon is reduced, the possibility of molecular weight reduction caused by severe hydrolysis of polyester molecules in the spinning process can be reduced, the improvement of the fiber dyeing uniformity is facilitated, the whole process flow is short, and the production efficiency is high.

In conclusion, the invention has the following beneficial effects:

1. aerogel and DTY are combined to form the aerogel textile fabric with various characteristics of aerogel, the thermal conductivity of the aerogel textile fabric is lower than that of static air, and the thermal insulation performance of the aerogel textile fabric is far superior to that of common fibers. Meanwhile, the fabric has the characteristics of light weight, quick drying, peculiar smell resistance, easy dyeing and low static electricity;

2. the water in the sol is replaced by the ethanol, so that the liquid interface tension of the gel framework is reduced, the Si-OH on the surfaces of the pore channels of the sol is modified by the ethanol, the reaction between the Si-OH and water molecules in the air is prevented, and the loss of the pore structure of the aerogel can be reduced, so that the weight of the aerogel textile fabric is reduced, and the heat retention property is enhanced;

3. under the acidic condition, the gel time is prolonged, the sol particles are crosslinked and loosened to finally form three-dimensional molecular network sol, the flexibility and the folding resistance of the aerogel textile fabric are improved, the service life of the aerogel textile fabric is prolonged, the aerogel textile fabric can be made into sports wear which is attached to a human body, the unfolding action is facilitated, the aerogel textile fabric is light and warm, and the application range is enlarged.

Detailed Description

The present invention will be described in further detail with reference to examples.

The specification and source information of the raw materials and components involved in the present invention are shown in table 1.

Table 1 specification and source information for raw materials and components

Preparation example

Preparation example 1:

s1, washing the corn straws, primarily crushing the corn straws by a knife switch, drying the corn straws in an oven at 35 ℃, further crushing the corn straws by a crusher, removing large particles by a 40-mesh screen, and pouring the corn straws into a ball mill with the rotating speed of 400r/min for ball milling for 6 hours to obtain straw powder;

s2, adding 5 weight parts of straw powder to 120 weight parts of 4% H₂O₂And mixing the plant substrate and 15% NaOH composite aqueous solution, oscillating for 3h by a constant-temperature oscillator, filtering by a 200-mesh screen, washing a filter cake to be neutral by distilled water, and drying in a 55-DEG C oven to obtain the plant substrate.

Preparation example 2:

s1, adding petroleum base (naphthenic base crude oil), the plant base prepared in the preparation example 1 and polyester fiber into a reaction kettle, and heating until the mixture is completely melted to obtain polymer melt;

s2, cooling and solidifying the polymer melt, and cutting to obtain cut particles with the particle size of 3-5 mm;

s3, drying the cut pellets in a drying agent until the water content is 20ppm, performing melt spinning to prepare POY (pre-oriented yarn extraction), and then performing drawing and twisting to prepare DTY (draw textured yarn).

Preparation example 3:

the difference from preparation example 2 was that in the step s3, the pellets were dried to a water content of 22 ppm.

Preparation example 4:

the difference from preparation example 2 was that in the step s3, the pellets were dried to a water content of 30 ppm.

Examples

Example 1:

s1, adding tetraethoxysilane serving as a precursor into a reaction kettle, adding a three-dimensional nitrogen-doped carbon nanotube (N-CNT) aerogel catalyst, uniformly stirring by using a cylinder stirrer, adding 5% hydrochloric acid to adjust the pH value to 4, and reacting to generate sol with rheological property;

s2, spraying the obtained sol on the DTY (draw textured yarn) prepared in the preparation example 2 by a spraying machine, standing for 10h to obtain wet gel, and obtaining wet gel loaded DTY (draw textured yarn);

s3, sequentially adding ethanol to DTY (draw textured yarn) loaded with wet gel for alcohol-water replacement, then adding methyl trimethylsilane for hydrophobic reaction, and then adopting CO₂Performing supercritical drying as a medium to obtain aerogel modified DTY (draw textured yarn);

Example 2:

the difference from the example 1 is that in the step s1, the weight ratio of the precursors added into the reaction kettle is 2: 13, and tetraethoxysilane.

Example 3:

the difference from example 2 is that in the s1 step, the weight ratio of the polyamide to the tetraethoxysilane is 3.5: 13.

Example 4:

the difference from example 2 is that in the s1 step, the weight ratio of the polyamide to the tetraethoxysilane is 5: 13.

Example 5:

the difference from example 1 is that in the step of s1, pH was adjusted to 5.

Example 6:

the difference from example 1 is that in the step of s1, pH was adjusted to 6.

Example 7:

the difference from example 1 is that DTY obtained in preparation example 3 was added in s2 step.

Example 8:

the difference from example 1 is that in the s3 step, formaldehyde was added for solvent replacement.

Example 9:

the difference from example 1 is that in the step s3, the hydrophobic reaction is hydrophobically modified by methyl trimethylsilane, vinyl trimethylsilane and phenyl trimethoxysilane, the weight ratio of methyl trimethylsilane, vinyl trimethylsilane and phenyl trimethoxysilane is 3: 1: 8.

example 10:

the difference from example 9 is that in the s3 step, the weight ratio of methyltrimethylsilane, vinyltrimethylsilane and phenyltrimethoxysilane was 3: 4: 8.

example 11:

the difference from example 9 is that in the s3 step, the weight ratio of methyltrimethylsilane, vinyltrimethylsilane and phenyltrimethoxysilane was 3: 1: 11.

example 12:

the difference from example 1 is that in the step s3, the drying medium is ethanol.

Comparative example

Comparative example 1:

the difference from example 1 is that pH was adjusted to 1 in the s1 step.

Comparative example 2:

the difference from example 1 is that in the step of s1, pH was adjusted to 8.

Comparative example 3:

the difference from example 1 is that DTY obtained in preparation example 4 was used in the step of s 2.

Comparative example 4:

the difference from example 1 is that in the step of s4, the DTY prepared in preparation example 2 was directly used for weaving to obtain a textile fabric.

Comparative example 5:

the difference from example 1 is that in the step s2, wet gel was directly prepared without adding DTY; in the step s3, directly carrying out solvent replacement and hydrophobic reaction on wet gel in sequence, and then carrying out wire drawing and drying to obtain aerogel wires; in step s4, the fabric is prepared by spinning with aerogel filaments.

Performance testing

Test method

The performance test method of the aerogel textile fabrics prepared in the above examples and comparative examples is as follows:

1. weight: according to GB/T24218.1-2009 part 1 of test methods for textile nonwovens: determination of mass per unit area the weight of a test specimen in an area of 1 square meter is measured;

2. pore diameter: the pore size of the sample was tested using a pore size tester (TOPASPSM165, germany);

3. thermal resistance: the YG606G thermal resistance and wet resistance tester is used for testing the thermal resistance of the sample;

4. compression performance: the compression work of the test specimens was tested according to GB/T24442.2-2009 "determination of textile compression Properties".

Test results

The performance test results of the aerogel textile fabrics prepared in the above examples are shown in table 2.

Table 2 results of performance tests of aerogel textile fabrics prepared in the examples.

The performance test results of the aerogel textile fabrics prepared according to the above respective proportions are shown in table 3.

Table 3 results of performance tests on aerogel textile fabrics prepared according to various comparative examples.

From the above data it can be seen that:

1. compared with the comparative example 4 and the example 1, the fabric modified by the aerogel has the advantages that the weight is reduced compared with the fabric of the common yarns, the thermal resistance is increased, the heat preservation effect is increased, the compression work is increased, the capability of the fabric modified by the aerogel for resisting the pressure of shock waves is better, the folding resistance of the fabric can be improved, the service life is prolonged, the application range is improved, in addition, the average pore diameter of the fabric is far smaller than that of the fabric of the common yarns, densely distributed micro pores are formed between the fabrics, the fabric can make a contribution to weight reduction and heat preservation, peculiar smell can be absorbed, the air circulation is accelerated, the effects of quick drying and low static electricity are realized, and the fabric dyeing is facilitated due to the provision of dye attachment points.

2. Compared with the embodiment 1, the embodiment 2-4 shows that when the compound of the polyamide amine and the tetraethoxysilane is used as the precursor, the advantages of the polyamide amine and the tetraethoxysilane are complemented, compared with the condition that the tetraethoxysilane is used as the precursor alone, the weight of the prepared fabric is further reduced, the heat retention is further increased, in addition, the average pore diameter of the fabric is also reduced, the weight reduction and the heat retention of the fabric are favorably considered, and the embodiment 2-4 shows that the specific gravity change of the polyamide amine and the tetraethoxysilane has influence on various performances of the fabric.

3. Compared with the comparative example 2, the embodiment 1 and the embodiments 5 to 6 show that in the reaction kettle, due to the fact that the polyamide and the tetraethoxysilane are subjected to step-by-step gradually-decreased fractional hydrolysis reaction, hydrolysis products are mutually condensed to generate sol, the condensation polymerization reaction is slowed down under the acidic condition relative to the alkaline condition, the gelation time is prolonged, cross linking among sol particles is loosened, and finally three-dimensional molecular network-shaped sol is formed, so that the weight is reduced more, the pore diameter is reduced, the thermal resistance is increased, the heat retention property of the fabric is improved, the weight is reduced, and meanwhile, the compression work is increased, which indicates that the flexibility and the folding resistance of the aerogel textile fabric are improved, and the service life of the aerogel textile fabric is prolonged.

4. It can be seen from the comparison between example 1 and examples 5-6 and comparative example 1 that when the pH is in the range of 4-6, the acidic environment is suitable, and the promotion to various properties of the fabric is large, but when the pH is too large, the gelation time is too long, so that the sol particles are too loose, and the pores are too large, which is beneficial to weight reduction, and is not beneficial to heat preservation and deformation resistance.

5. Compared with the comparative example 3, the example 1 shows that when the water content in the grain is more than 25ppm, the softening point of the high polyester is too low, and the phenomenon of pore blocking due to loop knot exists, so that the weight of the fabric is increased firstly, the improvement of the dyeing uniformity of the fiber is not facilitated, the thermal resistance is reduced, and the polyester molecules are hydrolyzed violently in the spinning process, and the molecular weight is reduced.

6. Compared with example 1, it can be seen from example 7 that when the water content in the cut grains is less than 25ppm, the weight of the fabric is increased along with the increase of the water content in the cut grains, but the thermal resistance is also increased, which is beneficial to warm keeping.

7. Compared with the example 8, the solvent replacement is carried out by using the ethanol, the replacement rate of water is high, the liquid interfacial tension of the gel framework is reduced, the Si-OH on the surfaces of the pore channels of the sol is modified by the ethanol, the reaction between the Si-OH and water molecules in the air is blocked, and the loss of the pore structure of the aerogel can be reduced, so that the weight of the aerogel textile fabric is reduced, and the heat retention property is enhanced.

8. Compared with the example 1, the examples 9-11 show that the gel skeleton is subjected to hydrophobic modification by compounding the methyl trimethylsilane, the vinyl trimethylsilane and the phenyl trimethoxysilane, so that the pressure condition for drying the gel skeleton can be reduced, the damage of water vapor in the air to the gel skeleton is reduced, the average pore diameter is reduced, and the heat retention property of the aerogel textile fabric is improved.

9. As can be seen from the comparison of example 12 with example 1, since CO is present₂Compared with the critical temperature of ethanol, the method can reduce the process pressure, further reduce the average pore diameter and increase the heat retention.

10. The aerogel itself has too poor mechanical properties to be woven into a fabric, so the comparative example 5 does not produce a finished product at all.

The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.

Claims

1. The preparation method of the aerogel textile fabric is characterized by comprising the following steps of:

2. The method for preparing aerogel textile fabric according to claim 1, wherein in the step s3, the solvent replacement adopts ethanol to replace water in the sol.

3. The method for preparing the aerogel textile fabric according to claim 1, wherein in the step s3, the hydrophobic reaction is performed by hydrophobic modification with methyltrimethylsilane, vinyltrimethylsilane and phenyltrimethoxysilane, and the weight ratio of methyltrimethylsilane, vinyltrimethylsilane and phenyltrimethoxysilane is 3: (1-4): (8-11).

4. The method for preparing the aerogel textile fabric according to claim 1, wherein in the step s1, the precursor comprises polyamide amine and tetraethoxysilane, and the weight ratio of the polyamide amine to the tetraethoxysilane is (2-5): 13.

5. the method of claim 1, wherein in the step of s1, the pH is adjusted to 4-6.

6. Method for preparing an aerogel textile fabric according to claim 1, which comprisesCharacterized in that in the step s3, CO is used for drying₂As a medium.

7. The method for preparing aerogel textile fabric according to claim 1, wherein in the step of s2, the DTY (draw textured yarn) preparation method comprises the following steps:

s2, cooling and solidifying the polymer melt, and cutting to obtain granules;

8. Aerogel textile fabric, characterized in that it is produced by the method of any one of claims 1 to 7.