阅读说明：本技术 一种类似羽绒功能的织物保暖填充材料及其制备方法和应用 (Fabric warm-keeping filling material with down-like function and preparation method and application thereof ) 是由 周凡雨 彭雄义 刘仰硕 董雄伟 李强 蔡亚君 彭其安 董会杰 张圣祖 吕少仿 于 2021-06-28 设计创作，主要内容包括：本发明涉及一种类似羽绒功能的织物保暖填充材料及其制备方法和应用。本发明将蚕丝溶解,制得混合溶液；将混合溶液浸入丙醇制得湿凝胶,将湿凝胶中的溶剂进行置换,然后干燥,制得柔性蚕丝气凝胶,即为类似羽绒功能的织物保暖填充材料；将织物保暖填充材料置于两层聚酯纤维面料中间,用针线进行缝合,将织物保暖填充材料包裹于聚酯纤维面料,制得的柔性蚕丝气凝胶的保暖面料。本发明制备的蚕丝气凝胶无需添加柔软剂等其他改性剂,其表现了很好的柔性,其可用于保暖衣的填充物。本发明将蚕丝制备为气凝胶,用于保暖衣的填充物,拓宽了蚕丝的新用途,具有很好的应用推广前景。(The invention relates to a fabric warm-keeping filling material with a down-like function, and a preparation method and application thereof. Dissolving silk to prepare a mixed solution; soaking the mixed solution into propanol to prepare wet gel, replacing the solvent in the wet gel, and then drying to prepare flexible silk aerogel, namely the fabric thermal filling material with the down feather-like function; placing the fabric thermal filling material between the two layers of polyester fiber fabric, sewing with needles and threads, and wrapping the fabric thermal filling material on the polyester fiber fabric to obtain the thermal fabric of the flexible silk aerogel. The silk aerogel prepared by the invention does not need other modifiers such as a softening agent and the like, shows good flexibility, and can be used as a filler of thermal clothes. The silk is prepared into the aerogel and used as the filler of the thermal clothes, so that the novel application of the silk is widened, and the application and popularization prospects are good.)

1. A preparation method of a fabric warm-keeping filling material with a down-like function is characterized by comprising the following steps:

(1) dissolving silk: taking appropriate amount of silk to a round bottom flask, adding CaCl dissolved in the silk₂Continuously stirring the mixed solution of ethanol and water for 3-5 hours at the temperature of 60-80 ℃ on a constant-temperature electromagnetic stirrer, and completely dissolving the silk to prepare a mixed solution;

(2) preparation of wet gel: pouring the mixed solution dissolved with the silk into a mold, and immersing the mold into propanol for gelling, wherein the gelling time is 5-24 hours, so that the wet gel is formed; then immersing the wet gel into absolute ethyl alcohol for replacement; the replacement time is 3-4 days, and the absolute ethyl alcohol is replaced every day; preparing a wet gel;

(3) and (3) drying: freeze-drying the wet gel at-55 to-65 ℃ for 12 to 24 hours to obtain the flexible silk aerogel; namely a fabric warm-keeping filling material with the function similar to down feather.

2. The method for preparing the down-like fabric warm-keeping filling material according to claim 1, wherein the method comprises the following steps: CaCl in the mixed solution in the step (1)₂The molar ratio of ethanol to water is as follows: 0.1: 2-4: 8-10; the mass volume ratio of the silk to the water is as follows: 1g to (10-12) mL.

3. The method for preparing the down-like fabric warm-keeping filling material according to claim 1, wherein the method comprises the following steps: the size of the die in the step (2) is as follows: 800cm × 100cm × 3 cm.

4. A fabric warm-keeping filling material with the down-like function is characterized by being prepared by the preparation method of the fabric warm-keeping filling material with the down-like function according to any one of claims 1 to 3.

5. The application of the down-like functional fabric thermal filling material as claimed in claim 1, which is characterized in that the application method comprises the following steps: placing the fabric thermal filling material between the two layers of polyester fiber fabric, sewing with needles and threads, and wrapping the fabric thermal filling material on the polyester fiber fabric to obtain the thermal fabric of the flexible silk aerogel.

Technical Field

The invention belongs to the technical field of preparation of fabric warm-keeping filling materials, and particularly relates to a fabric warm-keeping filling material with a down-like function, and a preparation method and application thereof.

Background

The aerogel material is a light solid material with a nano porous network structure, and has the characteristics of high porosity, large specific surface area, ultralow density, low thermal conductivity coefficient and the like. The advent of aerogel was traced back to 1931, where Kistler, Stanford university, successfully produced silica aerogel for the first time using supercritical drying technology. The discovery of aerogels has been almost 90 years old to date. Aerogel has unique properties, which make it a focus of the study in the field of materials. There are many types of aerogels, and the aerogels under extensive study mainly comprise inorganic aerogel materials (e.g., SO)₂Aerogel, Al₂O₃Aerogel, carbon-based aerogel), polymeric aerogel materials (e.g.: resorcinol-formaldehyde polymeric aerogels), organic-inorganic composite aerogels. Different types of aerogel materials have different performance advantages, such as: the silicon aerogel has low density and better flame retardance, the carbon aerogel has better conductivity, and the polymer aerogel has advantages in the aspect of mechanical property and the like. Aerogel materialThe material has wide application and wide application prospect in the fields of catalysis, electronic devices, heat preservation, heat insulation, detectors and the like.

However, the unique network structure and high porosity of the aerogel also cause the defects of low strength, poor toughness, easy destruction of the nano-pore structure under the action of external force and the like, thereby greatly limiting the practical application of the aerogel. Therefore, overcoming the disadvantages of aerogels, and developing them from extremely brittle aerogels into flexible aerogel materials is of great significance for practical use. In recent years, many researchers at home and abroad have been working on the development of flexible aerogels. Significant results have been achieved by altering the raw materials or manufacturing processes, using reinforcements, or compounding with other materials in an attempt to alter the disadvantages of aerogels, such as being fragile and not capable of being bent. Flexible aerogels, as the name implies, mean aerogels with excellent flexibility, developed by improving the raw materials and the preparation processes, such as drying methods, etc., on the basis of the conventional preparation methods. How to define the flexible aerogel and the common aerogel, for the flexible aerogel, when the flexible aerogel is subjected to an external force, the flexible aerogel deforms; when the external force is removed, the original shape is recovered, the microstructure is not changed, and the common aerogel does not have the performance. In practical use, the flexible aerogel can reduce the complexity in manufacturing and installation, has the advantages of light weight, good thermal shock resistance and the like, and has incomparable advantages for the application of complex shapes.

Silk is a continuous long fiber, also called natural silk, which is a natural fiber and is formed by coagulation of a silk liquid secreted by a mature silkworm during cocooning. Humans use one of the earliest animal fibers. Silk is one of ancient Chinese civilization products, the invention of Chinese workers is a very early thing, and the imperial concubine snail ancestor which is handed over to Huangdi begins to teach and breed silkworms; there are many silks and many side-of-silk characters in the oracle bone inscription. According to archaeology, china has made silk threads, woven ribbons and simple silk fabrics from silk approximately 4700 years ago. Silk is used for weaving silk fabrics such as silk, fine silk fabrics, yarn, crape, silk, brocade, embroidery and the like in the period of business weeks. The silkworm includes silkworm, tussah silkworm, castor silkworm, cassava silkworm, willow silkworm, and wild silkworm. The silk thread drawn from a single cocoon is called cocoon silk. There is no research on the use of silk for aerogel production.

Silk is generally used as a filling material for quilts, and has a good warm-keeping effect. However, silk is not effective for filling clothes because silk is smooth and is not easily fixed in clothes. Therefore, in order to apply silk to clothes, it is necessary to modify the silk and prepare the silk into a material that can be easily molded with fabrics.

Disclosure of Invention

The invention aims to provide a fabric warm-keeping filling material with a down-like function, which aims to overcome the defects in the prior art.

The invention aims to provide a fabric warm-keeping filling material with a down-like function, which can be prepared by the following method: dissolving silk to prepare a mixed solution; and (3) soaking the mixed solution into propanol to prepare wet gel, replacing the solvent in the wet gel, and then drying to prepare the flexible silk aerogel, namely the fabric thermal filling material with the down feather-like function.

The invention also aims to provide a preparation method of the fabric warm-keeping filling material with the down-like function, which comprises the following steps:

(1) dissolving silk: taking appropriate amount of silk to a round bottom flask, adding CaCl dissolved in the silk₂Continuously stirring the mixed solution of ethanol and water for 3-5 hours at the temperature of 60-80 ℃ on a constant-temperature electromagnetic stirrer, and completely dissolving the silk to prepare a mixed solution;

(2) preparation of wet gel: pouring the mixed solution dissolved with the silk into a mold, and immersing the mold into propanol for gelling, wherein the gelling time is 5-24 hours, so that the wet gel is formed; then immersing the wet gel into absolute ethyl alcohol for replacement; the replacement time is 3-4 days, and the absolute ethyl alcohol is replaced every day; preparing a wet gel;

(3) and (3) drying: freeze-drying the wet gel at-55 to-65 ℃ for 12 to 24 hours to obtain the flexible silk aerogel; namely a fabric warm-keeping filling material with the function similar to down feather.

Preferably, CaCl in the mixed solution in the step (1)₂The molar ratio of ethanol to water is as follows: 0.1: 2-4: 8-10.

Preferably, the mass-to-volume ratio of the silk (g) to the water (mL) in the step (1) is as follows: 1: 10-12.

Preferably, the die size in step (2) is: 800cm × 100cm × 3cm (length × width × thickness).

The invention also aims to provide an application of the fabric warm-keeping filling material with the down-like function, and the application method comprises the following steps: placing the fabric thermal filling material between the two layers of polyester fiber fabric, sewing with needles and threads, and wrapping the fabric thermal filling material on the polyester fiber fabric to obtain the thermal fabric of the flexible silk aerogel.

The invention has the following remarkable advantages:

(1) the inventors of the present application have unexpectedly found that a mixed solution of dissolved silk can be wet gel in a propanol solvent, which provides a new method for preparing wet gel.

(2) The inventor of the application unexpectedly finds that the prepared silk aerogel does not need other modifiers such as a softening agent and the like, shows good flexibility, and can be used as a filler of thermal clothes.

(3) The silk is prepared into the aerogel and used as the filler of the thermal clothes, so that the new application of the silk is widened.

Drawings

Figure 1 a schematic representation of the fabric thermal filling material prepared in example 1.

Detailed Description

The examples described below illustrate the invention in detail.

Example 1

In this embodiment, the fabric warm-keeping filling material with the down-like function is prepared by the following method, including the following steps:

(1) dissolving silk: adding 14.7g of silk into a round-bottom flask, and adding 0.1mol of CaCl₂A mixed solution of 3mol of ethanol and 9mol of water; continuously stirring the mixture for 4 hours at 70 ℃ on a constant-temperature electromagnetic stirrer, and completely dissolving the silk to prepare a mixed solution;

(2) preparation of wet gel: pouring the mixed solution dissolved with the silk into a mould and immersing the mould into propanol for gelling, wherein the mould has the following dimensions: gelling time of 800cm × 100cm × 3cm for 12 hours to obtain wet gel; then immersing the wet gel into absolute ethyl alcohol for replacement; the replacement time is 3 days, and the absolute ethyl alcohol is replaced every day; preparing a wet gel;

(3) and (3) drying: freeze-drying the wet gel at-60 ℃ for 18 hours to obtain the flexible silk aerogel; namely, the fabric thermal filling material with the function similar to the down feather is shown in figure 1.

The application method of the fabric warm-keeping filling material with the down feather-like function comprises the following steps: placing the fabric thermal filling material between the two layers of polyester fiber fabric, sewing with needles and threads, wrapping the fabric thermal filling material on the polyester fiber fabric, and obtaining the thermal fabric a of the flexible silk aerogel.

Example 2

In this embodiment, the fabric warm-keeping filling material with the down-like function is prepared by the following method, including the following steps:

(1) dissolving silk: adding 14.4g silk into a round-bottom flask, adding 0.1mol CaCl₂A mixed solution of 2mol of ethanol and 8mol of water; continuously stirring the mixture for 4 hours at 70 ℃ on a constant-temperature electromagnetic stirrer, and completely dissolving the silk to prepare a mixed solution;

(2) preparation of wet gel: pouring the mixed solution dissolved with the silk into a mould and immersing the mould into propanol for gelling, wherein the mould has the following dimensions: gelling time of 800cm × 100cm × 3cm for 12 hours to obtain wet gel; then immersing the wet gel into absolute ethyl alcohol for replacement; the replacement time is 3 days, and the absolute ethyl alcohol is replaced every day; preparing a wet gel;

(3) and (3) drying: freeze-drying the wet gel at-60 ℃ for 18 hours to obtain the flexible silk aerogel; namely a fabric warm-keeping filling material with the function similar to down feather.

The application method of the fabric warm-keeping filling material with the down feather-like function comprises the following steps: and (3) placing the fabric thermal filling material between the two layers of polyester fiber fabric, sewing with needles and threads, and wrapping the fabric thermal filling material on the polyester fiber fabric to obtain the thermal fabric b of the flexible silk aerogel.

Example 3

In this embodiment, the fabric warm-keeping filling material with the down-like function is prepared by the following method, including the following steps:

(1) dissolving silk: taking 15g of silk into a round-bottom flask, adding 0.1mol of CaCl₂A mixed solution of 4mol of ethanol and 10mol of water; continuously stirring the mixture for 4 hours at 70 ℃ on a constant-temperature electromagnetic stirrer, and completely dissolving the silk to prepare a mixed solution;

(2) preparation of wet gel: pouring the mixed solution dissolved with the silk into a mould and immersing the mould into propanol for gelling, wherein the mould has the following dimensions: gelling time of 800cm × 100cm × 3cm for 12 hours to obtain wet gel; then immersing the wet gel into absolute ethyl alcohol for replacement; the replacement time is 3 days, and the absolute ethyl alcohol is replaced every day; preparing a wet gel;

(3) and (3) drying: freeze-drying the wet gel at-60 ℃ for 18 hours to obtain the flexible silk aerogel; namely a fabric warm-keeping filling material with the function similar to down feather.

The application method of the fabric warm-keeping filling material with the down feather-like function comprises the following steps: and placing the fabric thermal filling material between the two layers of polyester fiber fabric, sewing with needles and threads, and wrapping the fabric thermal filling material on the polyester fiber fabric to obtain the thermal fabric c of the flexible silk aerogel.

Comparative example 1

In this comparative example, "0.1 mol of CaCl in step (1) was used in the preparation₂"adjusted to" 0.01mol CaCl₂"; other preparation methods and application methods are implemented with reference to example 1, and the prepared thermal fabric d of the flexible silk aerogel is obtained.

Comparative example 2

In this comparative example, "the gelation time was 12 hours" in the step (2) was adjusted to "the gelation time was 1.2 hours" in the production process; other preparation methods and application methods were carried out with reference to example 1, and a flexible silk aerogel thermal fabric e was obtained.

Comparative example 3

In this comparative example, "the wet gel frozen at-60 ℃" in step (3) was adjusted to "the wet gel frozen at-6 ℃ during the preparation process"; other preparation methods and application methods are implemented with reference to example 1, and the prepared thermal fabric f of the flexible silk aerogel is obtained.

Test example:

the thermal insulation performance of the thermal insulation fabrics a, b, c, d, e and f of the flexible silk aerogel prepared in the examples 1-3 and the comparative examples 1-3 is tested, the test method refers to GBT 18398 and 2001 clothing thermal resistance test method thermal body warming dummy method, and the test results are as follows:

item	Warm keeping fabric a	Warm keeping fabric b	Warm keeping fabric c	Warm keeping fabric d	Warm keeping fabric e	Warm keeping fabric f	Down jacket purchased in market
								Crohn value (clo)	0.66	0.68	0.71	0.42	0.46	0.47	0.45

The higher the Crohn value is, the better the thermal resistance is and the better the heat preservation performance is. According to the Crohn value in the table, the thermal fabric of the flexible silk aerogel prepared by the embodiment of the invention has excellent thermal insulation performance. The results of the comparative example show that: CaCl₂The dosage, the gelation time and the wet gel freezing temperature of the silk aerogel have important influence on the thermal insulation performance of the thermal insulation fabric of the silk aerogel.