Lightweight warm-keeping polyester wadding material and preparation method thereof

Abstract

The invention relates to the technical field of fabric spinning, and discloses a lightweight warm-keeping polyester wadding material and a preparation method thereof. The preparation method comprises the following steps: firstly, reacting 3, 5-dihydroxybenzamide with dicarboxyl polyethylene glycol to prepare polyethylene glycol amide polyester containing acylamino and polyethylene glycol chain segments; modifying cellulose aerogel by using the polyester, and finally blending the modified aerogel and PET (Polyethylene Terephthalate) to obtain the target polyester wadding. In the polyester, an amido bond and a hydroxyl group on the surface of the cellulose aerogel can form a hydrogen bond and partial covalent crosslinking, and an ether bond is similar to a PET ester group structure, so that the dispersity and compatibility of the modified aerogel in PET can be improved, and the flexibility of the PET can also be enhanced. The cellulose aerogel is porous, loose and small in heat conductivity coefficient, air convection can be limited, a heat conduction path is prolonged, heat loss is reduced, and finally the requirements for light weight and heat preservation of the polyester wadding are met.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of fabric spinning, in particular to a light and warm spray glue cotton material and a preparation method thereof. BACKGROUND

[0002] Spray glue cotton, also known as space cotton or vacuum cotton, is a kind of non-woven fabric. In the traditional process, the fiber raw material is carded into a single-layer thin net, and then is laid into a flake. The contact points between the fibers are bonded by spraying adhesive on both sides of the flake, and then are dried and solidified. Because the material has more contact points and fewer bridging points, it has the characteristics of softness, softness and elasticity. In recent years, spray glue cotton has been widely used in various aspects of people's life, mainly used in home clothes, which can meet the user's demand for soft and light home clothes. However, the existing spray glue cotton material is usually thick and not light, and solving this problem is the focus of current research.

[0003] The commonly used spray glue cotton raw material fiber is polyester fiber, which has the advantages of good wrinkle resistance and shape retention, high strength and elastic recovery ability, and is durable, wrinkle-free, and non-sticky. However, the polyester fiber has no hydrophilic group in the internal macromolecule, and has low moisture absorption and permeability, so the comfort of the finished garment is poor, and it is not soft enough to touch. And its performance in heat preservation and insulation is also lacking. Making polyester fiber warm and skin-friendly and soft is also a major direction of polyester fiber improvement.

[0004] Aerogel material has the basic characteristics of porosity, lightness, looseness and low thermal conductivity, which can slow down the speed of heat conduction, so as to achieve the purpose of isolating the transmission of heat and reducing the loss of heat. It is a kind of excellent thermal insulation material. Cellulose aerogel has the advantages of high surface area, high porosity, low thermal conductivity and low density. Adding it to polyester fiber can make polyester fiber have the characteristics of lightness, warmth and thermal insulation. SUMMARY

[0005] (I) Technical problems solved:

[0006] In view of the shortcomings of the prior art, the present application provides a light and warm spray glue cotton material and a preparation method thereof, which solves the problems of insufficient warmth and softness of traditional spray glue cotton.

[0007] (II) Technical scheme: The preparation method of the light and warm spray glue cotton material is as follows:

[0008] Step (1), 15.3-18.4 parts by weight of 3,5-dihydroxybenzamide and 100 parts by weight of double carboxyl polyethylene glycol are placed in a reaction bottle, anhydrous chloroform is added, nitrogen is introduced, then a solution containing 41.2-45.3 parts by weight of dicyclohexyl carbodiimide in chloroform is added, stirring at 20-25℃ for 1-3h, filtering, adding ethanol to precipitate, filtering, washing with ethanol, drying to obtain a polyethylene glycol amide polyester.

[0009] Step (2), the cellulose aerogel and the polyethylene glycol amide polyester are placed in water, ultrasonic dispersion and stirring at room temperature, filtering, washing with water and ethanol, drying to obtain a polyester modified aerogel.

[0010] Step (3), 100 parts by weight of PET is dried in a vacuum at 120-150℃ for 12-20h, then 0.2-1 parts by weight of polyester modified aerogel is added, mixed uniformly in a mixer, then added to the barrel of a twin-screw extruder, extruded, pelletized, then melt spun in a melt spinning machine, drawn to obtain a modified polyester fiber, woven, sprayed with adhesive, dried, cured to obtain a light weight and warm sprayed cotton material.

[0011] Further, the stirring time in step (2) is 3-6h.

[0012] Further, the amount of cellulose aerogel used in step (2) is 100 parts by weight, and the amount of polyethylene glycol amide polyester is 30-150 parts by weight.

[0013] Further, in step (3), the temperature of zone 1-5 of the screw extruder is 240-265℃, and the screw rotation speed is 50-120r / min.

[0014] Further, in step (3), the temperature of zone 1-4 of the melt spinning machine is 285-300℃, the spinning speed is 600-1000m / min, and the draw ratio is 3-3.5 times.

[0015] Further, in step (3), the curing temperature is 80-100℃, and the curing time is 8-15min.

[0016] (Three) beneficial technical effects:

[0017] The present application uses 3,5-dihydroxybenzamide and double carboxyl polyethylene glycol to react to obtain polyethylene glycol amide polyester, which is used to modify cellulose aerogel, and then the modified aerogel is blended and processed with PET to obtain a flexible and light weight spray glue cotton material with heat preservation performance. The hydroxyl groups at both ends of 3,5-dihydroxybenzamide react with the carboxyl groups at both ends of double carboxyl polyethylene glycol to form a polyester containing both amide groups and polyethylene glycol segments. The polyester forms hydrogen bonds and partial covalent cross-linking with the surface hydroxyl groups of the cellulose aerogel through amide bonds, firmly coating the cellulose aerogel, avoiding aerogel agglomeration, and improving the compatibility of the modified cellulose aerogel with PET. The polyethylene glycol segment contains abundant ether bonds, which are similar to the ester group structure of PET, improving the dispersibility of the modified cellulose aerogel in polyester fibers and the flexibility of the polyester fibers. The cellulose aerogel material has the basic characteristics of being porous, light, loose, and having a small thermal conductivity, a high surface area, and a low density. It can limit air convection and extend the heat conduction path to achieve the purpose of isolating heat transfer and reducing heat loss. It is an excellent thermal insulation material. Adding it to the spray glue cotton polyester fiber improves the thermal insulation performance of the spray glue cotton material while reducing its weight, meeting the lightweight and warm-keeping requirements of the spray glue cotton material. DETAILED DESCRIPTION

[0018] To make the objectives, technical solutions, and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be described clearly and completely below. If specific conditions are not specified in the embodiments, conventional conditions or manufacturer recommended conditions are used. If the reagents or instruments used are not specified by the manufacturer, they are all conventional products that can be purchased on the market.

[0019] The double carboxyl polyethylene glycol used in the present application has a molecular weight of 1000 and a model number of source leaf S28524 from Shanghai Source Leaf Biotechnology Co., Ltd.

[0020] Embodiment 1

[0021] (1) 30.6g of 3,5-dihydroxybenzamide (0.2mol) and 200g of double carboxyl polyethylene glycol were placed in a reaction bottle, 500mL of anhydrous chloroform was added, nitrogen was introduced, then 250mL of a solution of 82.4g of dicyclohexyl carbodiimide in chloroform was added, and the reaction was stirred at 25℃ for 3h, then filtered, the filtrate was precipitated by adding ethanol, filtered, washed with ethanol, and dried to obtain polyethylene glycol amide polyester.

[0022] (2) 20g of cellulose aerogel and 30g of polyethylene glycol amide polyester were placed in water, ultrasonically dispersed and stirred at room temperature for 3h, then filtered, washed with water and ethanol, and dried to obtain polyester modified aerogel.

[0023] (3), 2 kg of PET is cut into granules and dried in vacuum at 150 °C for 12 h, then 4 g of polyester modified aerogel is added, mixed uniformly in a mixer, extruded in a screw extruder, the temperature of 1-5 zones is 240 °C, 250 °C, 260 °C, 265 °C, 265 °C, the granules are cut, the screw rotation speed is 120 r / min, then melt spinning is carried out in a melt spinning machine at a speed of 600 m / min, the temperature of 1-4 zones is 285 °C, 295 °C, 295 °C, 300 °C, after spinning, drawing is carried out, the multiple is 3.5 times, modified polyester fiber is obtained, then drying and curing is carried out at 80 °C for 15 min, light weight and warm spray cotton material is obtained.

[0024] Example 2:

[0025] (1), 36.8 g of 3,5-dihydroxybenzamide and 200 g of double carboxyl polyethylene glycol are placed in a reaction bottle, 550 mL of anhydrous chloroform is added, nitrogen is introduced, then 200 mL of a solution containing 90.6 g of dicyclohexyl carbodiimide in chloroform is added, stirring is carried out at 20 °C for 1 h, filtration is carried out, the filtrate is precipitated by adding ethanol, filtration is carried out, ethanol washing is carried out, drying is carried out, and polyethylene glycol amide polyester is obtained.

[0026] (2), 20 g of cellulose aerogel and 6 g of polyethylene glycol amide polyester are placed in water, ultrasonic dispersion and stirring are carried out at room temperature for 6 h, filtration is carried out, washing is carried out with water and ethanol, drying is carried out, and polyester modified aerogel is obtained.

[0027] (3), 2 kg of PET is cut into granules and dried in vacuum at 120 °C for 20 h, then 10 g of polyester modified aerogel is added, mixed uniformly in a mixer, extruded in a screw extruder, the temperature of 1-5 zones is 240 °C, 250 °C, 260 °C, 265 °C, 265 °C, the granules are cut, the screw rotation speed is 50 r / min, then melt spinning is carried out in a melt spinning machine at a speed of 1000 m / min, the temperature of 1-4 zones is 285 °C, 295 °C, 295 °C, 300 °C, after spinning, drawing is carried out, the multiple is 3 times, modified polyester fiber is obtained, then drying and curing is carried out at 100 °C for 8 min, light weight and warm spray cotton material is obtained.

[0028] Example 3:

[0029] (1), 32.3 g of 3,5-dihydroxybenzamide and 200 g of double carboxyl polyethylene glycol are placed in a reaction bottle, 520 mL of anhydrous chloroform is added, nitrogen is introduced, then 230 mL of a solution containing 85.6 g of dicyclohexyl carbodiimide in chloroform is added, stirring is carried out at 25 °C for 3 h, filtration is carried out, the filtrate is precipitated by adding ethanol, filtration is carried out, ethanol washing is carried out, drying is carried out, and polyethylene glycol amide polyester is obtained.

[0030] (2), 20 g of cellulose aerogel and 12 g of polyester modified aerogel were put into water, ultrasonic dispersion and stirring for 4 h at room temperature, filtration, washing with water and ethanol, drying, to obtain polyester modified aerogel.

[0031] (3), 2 kg of PET was cut into granules and dried in vacuum at 130 °C for 15 h, then 15 g of polyester modified aerogel was added, mixed uniformly in a mixer, extruded in a screw extruder, the temperature of 1-5 zones was 240 °C, 250 °C, 260 °C, 265 °C, 265 °C, the granules were cut, the screw rotation speed was 100 r / min, then melt spinning was carried out in a melt spinning machine at a speed of 800 m / min, the temperature of 1-4 zones was 285 °C, 295 °C, 295 °C, 300 °C, drawing was carried out after spinning, the draw ratio was 3 times, to obtain modified polyester fiber, then drying and curing was carried out at 90 °C for 10 min, to obtain lightweight and warm spray cotton material.

[0032] Example 4:

[0033] (1), 35.6 g of 3,5-dihydroxybenzamide and 200 g of double carboxyl polyethylene glycol were put into a reaction bottle, 530 mL of anhydrous chloroform was added, nitrogen was introduced, then 225 mL of a solution containing 88.7 g of dicyclohexyl carbodiimide in chloroform was added, stirring was carried out at 20 °C for 1 h, filtration was carried out, the filtrate was precipitated by adding ethanol, filtration was carried out, ethanol washing was carried out, drying was carried out, to obtain polyester modified aerogel.

[0034] (2), 20 g of cellulose aerogel and 25 g of polyester modified aerogel were put into water, ultrasonic dispersion and stirring for 5 h at room temperature, filtration was carried out, washing with water and ethanol was carried out, drying was carried out, to obtain polyester modified aerogel.

[0035] (3), 2 kg of PET was cut into granules and dried in vacuum at 145 °C for 18 h, then 20 g of polyester modified aerogel was added, mixed uniformly in a mixer, extruded in a screw extruder, the temperature of 1-5 zones was 240 °C, 250 °C, 260 °C, 265 °C, 265 °C, the granules were cut, the screw rotation speed was 80 r / min, then melt spinning was carried out in a melt spinning machine at a speed of 750 m / min, the temperature of 1-4 zones was 285 °C, 295 °C, 295 °C, 300 °C, drawing was carried out after spinning, the draw ratio was 3.5 times, to obtain modified polyester fiber, then drying and curing was carried out at 85 °C for 12 min, to obtain lightweight and warm spray cotton material.

[0036] Comparative Example 1:

[0037] (1), 2 kg of PET was cut into granules and dried in vacuum at 150 °C for 12 h, then 4 g of cellulose aerogel was added, mixed uniformly in a mixer, and extruded in a screw extruder, with the temperature of 1-5 zones being 240 °C, 250 °C, 260 °C, 265 °C, 265 °C, the granules were cut, the screw rotation speed was 120 r / min, then melt spinning was performed in a melt spinning machine at a speed of 600 m / min, with the temperature of 1-4 zones being 285 °C, 295 °C, 295 °C, 300 °C, drawing was performed after spinning, the draw ratio was 3.5 times, polyester fibers were obtained, then drying and curing were performed at 80 °C for 15 min, and a spray glue cotton material was obtained.

[0038] Comparative Example 2:

[0039] (1), 20 g of cellulose aerogel and 30 g of 3,5-dihydroxybenzamide were put into water, ultrasonic dispersion and stirring were performed at room temperature for 3 h, filtration was performed, washing was performed with water and ethanol, and drying was performed, to obtain modified aerogel.

[0040] (2), 2 kg of PET was cut into granules and dried in vacuum at 150 °C for 12 h, then 4 g of modified aerogel was added, mixed uniformly in a mixer, and extruded in a screw extruder, with the temperature of 1-5 zones being 240 °C, 250 °C, 260 °C, 265 °C, 265 °C, the granules were cut, the screw rotation speed was 120 r / min, then melt spinning was performed in a melt spinning machine at a speed of 600 m / min, with the temperature of 1-4 zones being 285 °C, 295 °C, 295 °C, 300 °C, drawing was performed after spinning, the draw ratio was 3.5 times, polyester fibers were obtained, then drying and curing were performed at 80 °C for 15 min, and a spray glue cotton material was obtained.

[0041] Comparative Example 3:

[0042] (1), 20 g of cellulose aerogel and 30 g of carboxyl-terminated polyethylene glycol were put into water, ultrasonic dispersion and stirring were performed at room temperature for 3 h, filtration was performed, washing was performed with water and ethanol, and drying was performed, to obtain modified aerogel.

[0043] (2), 2 kg of PET was cut into granules and dried in vacuum at 150 °C for 12 h, then 4 g of modified aerogel was added, mixed uniformly in a mixer, and extruded in a screw extruder, with the temperature of 1-5 zones being 240 °C, 250 °C, 260 °C, 265 °C, 265 °C, the granules were cut, the screw rotation speed was 120 r / min, then melt spinning was performed in a melt spinning machine at a speed of 600 m / min, with the temperature of 1-4 zones being 285 °C, 295 °C, 295 °C, 300 °C, drawing was performed after spinning, the draw ratio was 3.5 times, polyester fibers were obtained, then drying and curing were performed at 80 °C for 15 min, and a spray glue cotton material was obtained.

[0044] Comparative Example 4:

[0045] (1) Put 22.2 g of resorcinol (0.2 mol) and 200 g of double carboxyl polyethylene glycol into a reaction bottle, add 500 mL of anhydrous chloroform, pass nitrogen, then add 250 mL of a solution of 82.4 g of dicyclohexyl carbodiimide in chloroform, stir at 25°C for 3 h, filter, add ethanol to precipitate, filter, wash with ethanol, and dry to obtain polyethylene glycol phenyl ring polyester.

[0046] (2) Put 20 g of cellulose aerogel and 30 g of polyethylene glycol phenyl ring polyester into water, ultrasonically disperse and stir at room temperature for 3 h, filter, wash with water and ethanol, and dry to obtain the aerogel.

[0047] (3) Cut 2 kg of PET into granules, dry in vacuum at 150°C for 12 h, then add 4 g of aerogel, mix uniformly in a mixer, extrude in a screw extruder, the temperature of 1-5 zones is 240°C, 250°C, 260°C, 265°C, 265°C, cut into granules, the screw rotation speed is 120 r / min, then melt-spinning in a melt spinning machine at a speed of 600 m / min, the temperature of 1-4 zones is 285°C, 295°C, 295°C, 300°C, after spinning, draw at a draw ratio of 3.5 times, to obtain polyester fiber, then dry and solidify at 80°C for 15 min to obtain the spray cotton material.

[0048] Determination of the initial modulus and elongation at break of the fiber: test according to GB / T 14337-2022 "Chemical fiber short fiber tensile property test method".

[0049] Test of the surface density of the fabric: test according to the test method of GB / T 24218.1-2009 "Textiles - Test methods for nonwovens - Part 1: determination of the mass per unit area".

[0050] Determination of the thermal resistance of the fabric: test according to the test method of standard GB / T 11048-2018 "Textiles - Physiological comfort - Determination of thermal resistance and vapor permeability (evaporative heat panel method)".

[0051] Table 1 Performance test of the spray cotton material

[0052]

[0053]

[0054] In Examples 1-4, 3,5-dihydroxybenzamide and double carboxyl polyethylene glycol are used to obtain polyethylene glycol amide polyester, the cellulose aerogel is modified by the polyethylene glycol amide polyester, and the obtained modified aerogel is blended and processed with PET to obtain a flexible, light and warm spray cotton material. The hydroxyl groups at both ends of 3,5-dihydroxybenzamide react with the carboxyl groups at both ends of double carboxyl polyethylene glycol to form a polyester containing amide groups and polyethylene glycol segments. The polyester forms hydrogen bonds and partial covalent cross-linking with the surface hydroxyl groups of the cellulose aerogel through amide bonds, firmly coating the cellulose aerogel, avoiding aerogel agglomeration, and improving the compatibility of the modified cellulose aerogel with PET. The polyethylene glycol segment contains abundant ether bonds, which are similar to the ester groups of PET, improving the dispersibility of the modified cellulose aerogel in polyester fibers and the flexibility of the polyester fibers. The cellulose aerogel material has basic properties such as porosity, lightness, looseness, low thermal conductivity, high surface area and low density, and can limit air convection and extend the heat conduction path to achieve the purpose of isolating heat transfer and reducing heat loss. It is an excellent thermal insulation material, and its addition to the spray cotton polyester fiber improves the thermal insulation performance of the spray cotton material while reducing its weight, achieving the lightweight and warm demand of the spray cotton material.

[0055] In Comparative Example 1, the cellulose aerogel is not modified, so its dispersibility in polyester fibers cannot be improved, and it is prone to agglomeration, which makes it difficult to optimize the performance of polyester fibers.

[0056] In Comparative Example 2, only 3,5-dihydroxybenzamide is used to react with the cellulose aerogel. Although the amide groups in the molecule can achieve the adhesion of the aerogel, the compatibility with PET is poor because the polyester structure is not formed.

[0057] In Comparative Example 3, carboxyl-terminated polyethylene glycol is used to modify the cellulose aerogel. Since the carboxyl-terminated polyethylene glycol molecule contains ether bonds, and the structure is similar to that of PET, the compatibility of the aerogel with PET is improved to some extent, and the influence on the performance of polyester fibers is reduced.

[0058] In Comparative Example 4, the polyester obtained by the reaction of resorcinol and double carboxyl polyethylene glycol is used to modify the cellulose aerogel. However, the polyester molecule does not contain amide bonds, and cannot form stable bonds with the cellulose aerogel, which is easily eluted during subsequent washing, so it cannot modify the aerogel.

[0059] It should be understood that the examples are only used for illustrating the present application and are not intended to limit the scope of protection of the present application. Furthermore, it should also be understood that after reading the technical content of the present application, those skilled in the art can make various modifications, changes or variations to the present application, and all these equivalent forms are also within the scope of protection defined by the appended claims.

Claims

1. A method for preparing a lightweight, heat-insulating spray-bonded cotton material, characterized in that, The preparation method is as follows: Step (1): Place 3,5-dihydroxybenzamide and dicarboxylated polyethylene glycol in a reaction flask, add anhydrous chloroform, purge with nitrogen, then add a chloroform solution containing dicyclohexylcarbodiimide, stir to react, filter, add ethanol to the filtrate for precipitation, filter, wash with ethanol, and dry to obtain polyethylene glycol amide polyester. Step (2): Place cellulose aerogel and polyethylene glycol amide polyester in water, ultrasonically disperse and stir at room temperature, filter, wash with water and ethanol, and dry to obtain polyester modified aerogel; Step (3): Cut 100 parts by weight of PET into pellets and vacuum dry them at 120-150℃ for 12-20h. Then add 0.2-1 parts by weight of polyester modified aerogel, mix them evenly in a mixer, and then add them to the barrel of a twin-screw extruder. Extrude and pelletize them, then melt spin them in a melt spinning machine, stretch them, and obtain modified polyester fibers. Weave them into a web, spray adhesive, dry them, and cure them to obtain a lightweight and warm spray-bonded cotton material.

2. The method for preparing the lightweight, heat-insulating spray-bonded cotton material according to claim 1, characterized in that, In step (1), the amount of 3,5-dihydroxybenzamide used is 15.3-18.4 parts by weight, the amount of dicarboxylated polyethylene glycol used is 100 parts by weight, and the amount of dicyclohexylcarbodiimide used is 41.2-45.3 parts by weight.

3. The method for preparing the lightweight, heat-insulating spray-bonded cotton material according to claim 1, characterized in that, The temperature of the stirring reaction in step (1) is 20-25℃, and the stirring reaction time is 1-3h.

4. The method for preparing the lightweight, heat-insulating spray-bonded cotton material according to claim 1, characterized in that, The stirring time in step (2) is 3-6 hours.

5. The method for preparing the lightweight, heat-insulating spray-bonded cotton material according to claim 1, characterized in that, In step (2), the amount of cellulose aerogel used is 100 parts by weight, and the amount of polyethylene glycol amide polyester used is 30-150 parts by weight.

6. The method for preparing the lightweight, heat-insulating spray-bonded cotton material according to claim 1, characterized in that, In step (3), the temperature of zones 1-5 of the screw extruder is 240-265℃, and the screw speed is 50-120r / min.

7. The method for preparing the lightweight, heat-insulating spray-bonded cotton material according to claim 1, characterized in that, In step (3), the temperature of zones 1-4 of the melt spinning machine is 285-300℃, the spinning speed is 600-1000m / min, and the draw ratio is 3-3.5 times.

8. The method for preparing the lightweight, heat-insulating spray-bonded cotton material according to claim 1, characterized in that, In step (3), the curing temperature is 80-100℃ and the curing time is 8-15min.

9. A lightweight, heat-insulating spray-bonded cotton material prepared by the preparation method described in claims 1-8.

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