Lightweight warm adhesive cotton material and preparation method thereof

Abstract

The application relates to the technical field of fabric spinning, and discloses a light-weight and warm spray glue cotton material and a preparation method thereof. In the application, 3,5-dihydroxybenzamide is first reacted with double-carboxyl polyethylene glycol to prepare polyethylene glycol amide polyester containing amide groups and polyethylene glycol segments; then the polyester is used to modify cellulose aerogel; and finally, the modified aerogel is blended and processed with PET to obtain the target spray glue cotton. In the polyester, the amide bond can form hydrogen bonds and part of covalent cross-linking with the surface hydroxyl groups of the cellulose aerogel; the ether bond can improve the dispersibility and compatibility of the modified aerogel in the PET due to the similar structure of the ether bond and the PET ester group, and can also enhance the flexibility of the PET. The cellulose aerogel is porous and loose, and has a small thermal conductivity, so that the air convection can be limited, the heat conduction path is prolonged, and the heat loss is reduced, and finally the light-weight and warm demand of the spray glue cotton is realized.

Description

Technical Field

[0001] This invention relates to the field of fabric spinning technology, specifically to a lightweight and warm spray-bonded cotton material and its preparation method. Background Technology

[0002] Spray-bonded cotton, also known as space cotton or vacuum cotton, is a type of nonwoven fabric. In traditional processes, fiber raw materials are carded into a single-layer thin web, then laid into sheets. Adhesive is sprayed onto both sides of the sheets, bonding the fiber junctions. After drying and curing, the material is formed. Because this type of material has many contact points and few bridging points, it possesses characteristics such as looseness, softness, and elasticity. In recent years, spray-bonded cotton has been widely used in various aspects of life, primarily in loungewear, satisfying users' desire for soft and lightweight loungewear. However, existing spray-bonded cotton materials are often quite thick and not lightweight; solving this problem is currently a hot research topic.

[0003] Polyester fiber is the most commonly used raw material for spray-bonded cotton. Its advantages include excellent wrinkle resistance and shape retention, high strength and elastic recovery, durability, wrinkle resistance, and non-pilling properties. However, polyester fibers lack hydrophilic groups in their macromolecules, resulting in low moisture absorption and permeability. Garments made from polyester are less comfortable to the touch and lack softness. Furthermore, its thermal insulation properties are somewhat lacking. Making polyester fibers both warm and soft against the skin is a major direction for improvement.

[0004] Aerogel materials possess fundamental characteristics such as porosity, lightness, looseness, and low thermal conductivity, which can slow down the rate of heat conduction, thereby achieving the purpose of isolating heat transfer and reducing heat loss. They are therefore high-performance thermal insulation materials. Cellulose aerogels have advantages such as high surface area, high porosity, low thermal conductivity, and low density. Adding them to polyester fibers can give the polyester fibers lightweight, heat-insulating, and thermal-resistant properties. Summary of the Invention

[0005] (a) Technical problems to be solved:

[0006] To address the shortcomings of existing technologies, this invention provides a lightweight and warm spray-bonded cotton material and its preparation method, solving the problems of insufficient warmth retention and lack of softness and lightness of traditional spray-bonded cotton.

[0007] (II) Technical Solution: The preparation method of lightweight and heat-insulating spray-bonded cotton material is as follows:

[0008] Step (1): Place 15.3-18.4 parts by weight of 3,5-dihydroxybenzamide and 100 parts by weight of dicarboxylated polyethylene glycol in a reaction flask, add anhydrous chloroform, purge with nitrogen, and then add a chloroform solution containing 41.2-45.3 parts by weight of dicyclohexylcarbodiimide. Stir the reaction at 20-25℃ for 1-3 hours, filter, add ethanol to the filtrate for precipitation, filter, wash with ethanol, and dry to obtain polyethylene glycol amide polyester.

[0009] 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.

[0010] 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.

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

[0012] Furthermore, 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.

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

[0014] Furthermore, 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.

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

[0016] (III) Beneficial Technical Effects:

[0017] This invention uses 3,5-dihydroxybenzamide and dicarboxylated polyethylene glycol to obtain polyethylene glycol amide polyester, which is used to modify cellulose aerogel. The modified aerogel is then blended with PET to obtain a flexible, lightweight, and heat-insulating spray-bonded cotton material. The hydroxyl groups at both ends of 3,5-dihydroxybenzamide react with the carboxyl groups at both ends of dicarboxylated polyethylene glycol to polymerize, generating a polyester containing both amide and polyethylene glycol segments. This polyester forms hydrogen bonds and partial covalent crosslinks with the hydroxyl groups on the surface of the cellulose aerogel through amide bonds, firmly encapsulating the cellulose aerogel, preventing aerogel aggregation and improving its compatibility with PET. The polyethylene glycol segments contain abundant ether bonds, similar to the ester structure of PET, improving the dispersibility of the modified cellulose aerogel in the polyester fiber and simultaneously increasing the flexibility of the polyester fiber. Cellulose aerogel materials possess basic characteristics such as being porous, lightweight, loose, having low thermal conductivity, high surface area, and low density. They can achieve the purpose of isolating heat transfer and reducing heat loss by restricting air convection and extending the heat conduction path. They are high-performance thermal insulation materials. Adding them to spray-bonded polyester fibers can improve the thermal insulation performance of spray-bonded cotton materials while reducing their weight, thus meeting the lightweight thermal insulation requirements of spray-bonded cotton materials. Detailed Implementation

[0018] To make the objectives, technical solutions, and advantages of the embodiments of this application clearer, the technical solutions in the embodiments of this application will be clearly and completely described below. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall apply. Reagents or instruments whose manufacturers are not specified are all conventional products that can be purchased commercially.

[0019] The present invention relates to dicarboxylated polyethylene glycol with a molecular weight of 1000, model number Yuanye S28524, manufactured by Shanghai Yuanye Biotechnology Co., Ltd.

[0020] Example 1:

[0021] (1) Place 30.6 g of 3,5-dihydroxybenzamide (0.2 mol) and 200 g of dicarboxylated polyethylene glycol in a reaction flask, add 500 mL of anhydrous chloroform, purge with nitrogen gas, and then add 250 mL of chloroform solution containing 82.4 g of dicyclohexylcarbodiimide. Stir the reaction at 25 °C for 3 h, filter, add ethanol to the filtrate for precipitation, filter, wash with ethanol, and dry to obtain polyethylene glycol amide polyester.

[0022] (2) Place 20g of cellulose aerogel and 30g of polyethylene glycol amide polyester in water, ultrasonically disperse and stir for 3h at room temperature, filter, wash with water and ethanol, and dry to obtain polyester modified aerogel.

[0023] (3) Cut 2kg of PET into pellets and vacuum dry them at 150℃ for 12h. Then add 4g of polyester modified aerogel and mix them evenly in a mixer. Extrude the pellets in a screw extruder with temperatures of 240℃, 250℃, 260℃, 265℃ and 265℃ in zones 1-5. Cut the pellets at a screw speed of 120r / min. Then melt spin the pellets in a melt spinning machine at a speed of 600m / min with temperatures of 285℃, 295℃, 295℃ and 300℃ in zones 1-4. After spinning, stretch the pellets to a ratio of 3.5 times to obtain modified polyester fibers. Then dry and cure the fibers at 80℃ for 15min to obtain a lightweight and warm spray-bonded cotton material.

[0024] Example 2:

[0025] (1) Place 36.8g of 3,5-dihydroxybenzamide and 200g of dicarboxylated polyethylene glycol in a reaction flask, add 550mL of anhydrous chloroform, purge with nitrogen, and then add 200mL of chloroform solution containing 90.6g of dicyclohexylcarbodiimide. Stir the reaction at 20℃ for 1h, filter, add ethanol to the filtrate for precipitation, filter, wash with ethanol, and dry to obtain polyethylene glycol amide polyester.

[0026] (2) 20g of cellulose aerogel and 6g of polyethylene glycol amide polyester were placed in water, ultrasonically dispersed and stirred for 6h at room temperature, filtered, washed with water and ethanol, and dried to obtain polyester modified aerogel.

[0027] (3) Cut 2kg of PET into pellets and vacuum dry them at 120℃ for 20h. Then add 10g of polyester modified aerogel and mix them evenly in a mixer. Extrude the pellets in a screw extruder with temperatures of 240℃, 250℃, 260℃, 265℃ and 265℃ in zones 1-5. Cut the pellets at a screw speed of 50r / min. Then melt spin them in a melt spinning machine at a speed of 1000m / min with temperatures of 285℃, 295℃, 295℃ and 300℃ in zones 1-4. After spinning, stretch the fibers by a factor of 3 to obtain modified polyester fibers. Then dry and cure the fibers at 100℃ for 8min to obtain a lightweight and warm spray-bonded cotton material.

[0028] Example 3:

[0029] (1) Place 32.3g of 3,5-dihydroxybenzamide and 200g of dicarboxylated polyethylene glycol in a reaction flask, add 520mL of anhydrous chloroform, purge with nitrogen, and then add 230mL of chloroform solution containing 85.6g of dicyclohexylcarbodiimide. Stir the reaction at 25℃ for 3h, filter, add ethanol to the filtrate for precipitation, filter, wash with ethanol, and dry to obtain polyethylene glycol amide polyester.

[0030] (2) 20g of cellulose aerogel and 12g of polyethylene glycol amide polyester were placed in water, ultrasonically dispersed and stirred for 4h at room temperature, filtered, washed with water and ethanol, and dried to obtain polyester modified aerogel.

[0031] (3) Cut 2kg of PET into pellets and vacuum dry them at 130℃ for 15h. Then add 15g of polyester modified aerogel and mix them evenly in a mixer. Extrude them in a screw extruder with temperatures of 240℃, 250℃, 260℃, 265℃ and 265℃ in zones 1-5. Cut the pellets and the screw speed is 100r / min. Then melt spin them in a melt spinning machine at a speed of 800m / min with temperatures of 285℃, 295℃, 295℃ and 300℃ in zones 1-4. After spinning, stretch them to a multiple of 3 to obtain modified polyester fibers. Then dry and cure them at 90℃ for 10min to obtain lightweight and warm spray-bonded cotton material.

[0032] Example 4:

[0033] (1) Place 35.6g of 3,5-dihydroxybenzamide and 200g of dicarboxylated polyethylene glycol in a reaction flask, add 530mL of anhydrous chloroform, purge with nitrogen, and then add 225mL of chloroform solution containing 88.7g of dicyclohexylcarbodiimide. Stir the reaction at 20℃ for 1h, filter, add ethanol to the filtrate for precipitation, filter, wash with ethanol, and dry to obtain polyethylene glycol amide polyester.

[0034] (2) Place 20g of cellulose aerogel and 25g of polyethylene glycol amide polyester in water, ultrasonically disperse and stir for 5h at room temperature, filter, wash with water and ethanol, and dry to obtain polyester modified aerogel.

[0035] (3) Cut 2kg of PET into pellets and vacuum dry them at 145℃ for 18h. Then add 20g of polyester modified aerogel and mix them evenly in a mixer. Extrude the pellets in a screw extruder at temperatures of 240℃, 250℃, 260℃, 265℃ and 265℃ in zones 1-5. Cut the pellets at a screw speed of 80r / min. Then melt spin them in a melt spinning machine at a speed of 750m / min at temperatures of 285℃, 295℃, 295℃ and 300℃ in zones 1-4. After spinning, stretch the fibers to a ratio of 3.5 times to obtain modified polyester fibers. Then dry and cure the fibers at 85℃ for 12min to obtain a lightweight and warm spray-bonded cotton material.

[0036] Comparative Example 1:

[0037] (1) Cut 2kg of PET into pellets and vacuum dry them at 150℃ for 12h. Then add 4g of cellulose aerogel and mix them evenly in a mixer. Extrude the pellets in a screw extruder at temperatures of 240℃, 250℃, 260℃, 265℃ and 265℃ in zones 1-5. Cut the pellets at a screw speed of 120r / min. Then melt spin them in a melt spinning machine at a speed of 600m / min at temperatures of 285℃, 295℃, 295℃ and 300℃ in zones 1-4. After spinning, stretch the fibers to a ratio of 3.5 times to obtain polyester fibers. Then dry and cure the fibers at 80℃ for 15min to obtain spray-bonded cotton material.

[0038] Comparative Example 2:

[0039] (1) 20g of cellulose aerogel and 30g of 3,5-dihydroxybenzamide were placed in water, ultrasonically dispersed and stirred for 3h at room temperature, filtered, washed with water and ethanol, and dried to obtain modified aerogel.

[0040] (2) Cut 2kg of PET into pellets and vacuum dry them at 150℃ for 12h. Then add 4g of modified aerogel and mix them evenly in a mixer. Extrude the pellets in a screw extruder at temperatures of 240℃, 250℃, 260℃, 265℃ and 265℃ in zones 1-5. Cut the pellets at a screw speed of 120r / min. Then melt spin them in a melt spinning machine at a speed of 600m / min at temperatures of 285℃, 295℃, 295℃ and 300℃ in zones 1-4. After spinning, stretch the fibers to a ratio of 3.5 times to obtain polyester fibers. Then dry and cure the fibers at 80℃ for 15min to obtain spray-bonded cotton material.

[0041] Comparative Example 3:

[0042] (1) Place 20g of cellulose aerogel and 30g of carboxyl-terminated polyethylene glycol in water, ultrasonically disperse and stir for 3h at room temperature, filter, wash with water and ethanol, and dry to obtain modified aerogel.

[0043] (2) Cut 2kg of PET into pellets and vacuum dry them at 150℃ for 12h. Then add 4g of modified aerogel and mix them evenly in a mixer. Extrude the pellets in a screw extruder at temperatures of 240℃, 250℃, 260℃, 265℃ and 265℃ in zones 1-5. Cut the pellets at a screw speed of 120r / min. Then melt spin them in a melt spinning machine at a speed of 600m / min at temperatures of 285℃, 295℃, 295℃ and 300℃ in zones 1-4. After spinning, stretch the fibers to a ratio of 3.5 times to obtain polyester fibers. Then dry and cure the fibers at 80℃ for 15min to obtain spray-bonded cotton material.

[0044] Comparative Example 4:

[0045] (1) Place 22.2g resorcinol (0.2mol) and 200g dicarboxylated polyethylene glycol in a reaction flask, add 500mL of anhydrous chloroform, purge with nitrogen, and then add 250mL of chloroform solution containing 82.4g of dicyclohexylcarbodiimide. Stir the reaction at 25℃ for 3h, filter, add ethanol to the filtrate for precipitation, filter, wash with ethanol, and dry to obtain polyethylene glycol benzene ring polyester.

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

[0047] (3) Cut 2kg of PET into pellets and vacuum dry them at 150℃ for 12h. Then add 4g of aerogel and mix them evenly in a mixer. Extrude the pellets in a screw extruder at temperatures of 240℃, 250℃, 260℃, 265℃ and 265℃ in zones 1-5. Cut the pellets at a screw speed of 120r / min. Then melt spin them in a melt spinning machine at a speed of 600m / min at temperatures of 285℃, 295℃, 295℃ and 300℃ in zones 1-4. After spinning, stretch the fibers to a ratio of 3.5 times to obtain polyester fibers. Then dry and cure the fibers at 80℃ for 15min to obtain spray-bonded cotton material.

[0048] Determination of initial modulus and elongation at break of fiber: Tested in accordance with GB / T 14337-2022 "Test Method for Tensile Properties of Chemical Fibers (Short Fibers)".

[0049] Fabric surface density test: determined according to the test method of GB / T 24218.1-2009 "Textiles - Test methods for nonwoven fabrics - Part 1: Determination of mass per unit area".

[0050] Fabric thermal resistance determination: The test method is determined according to the standard GB / T 11048-2018 "Determination of thermal and moisture resistance of textiles under steady-state conditions for physiological comfort (evaporative hot plate method)".

[0051] Table 1 Performance Tests of Spray-bonded Wool Materials

[0052]

[0053]

[0054] In Examples 1-4, polyethylene glycol amide polyester was obtained by reacting 3,5-dihydroxybenzamide and dicarboxylated polyethylene glycol. Cellulose aerogel was modified with this polyethylene glycol amide polyester, and then the modified aerogel was blended with PET to obtain a flexible, lightweight, and heat-insulating spray-bonded cotton material. The hydroxyl groups at both ends of 3,5-dihydroxybenzamide react with the carboxyl groups at both ends of dicarboxylated polyethylene glycol to polymerize, generating a polyester containing both amide and polyethylene glycol segments. This polyester forms hydrogen bonds and partial covalent crosslinks with the hydroxyl groups on the surface of the cellulose aerogel through amide bonds, firmly encapsulating the cellulose aerogel, preventing aerogel aggregation and improving its compatibility with PET. The polyethylene glycol segments contain abundant ether bonds, similar to the ester structure of PET, which improves the dispersibility of the modified cellulose aerogel in the polyester fiber and also enhances the flexibility of the polyester fiber. Cellulose aerogel materials possess basic characteristics such as being porous, lightweight, loose, having low thermal conductivity, high surface area, and low density. They can achieve the purpose of isolating heat transfer and reducing heat loss by restricting air convection and extending the heat conduction path. They are high-performance thermal insulation materials. Adding them to spray-bonded polyester fibers can improve the thermal insulation performance of spray-bonded cotton materials while reducing their weight, thus meeting the lightweight thermal insulation requirements of spray-bonded cotton materials.

[0055] In Comparative Example 1, no modification treatment was applied to the cellulose aerogel, which resulted in its dispersibility in polyester fibers not being improved, making it prone to agglomeration and thus unable to optimize the performance of polyester fibers.

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

[0057] In Comparative Example 3, carboxyl-terminated polyethylene glycol was used to modify cellulose aerogel. Since carboxyl-terminated polyethylene glycol contains ether bonds and its structure is similar to that of PET, it improves the compatibility of aerogel with PET to a certain extent and reduces the impact on the performance of polyester fibers.

[0058] In Comparative Example 4, a polyester generated by reacting resorcinol with dicarboxylated polyethylene glycol was used to modify cellulose aerogel. However, the polyester molecule does not contain amide bonds and cannot form a stable bond with cellulose aerogel. It is easily washed away during subsequent washing and thus cannot play the role of modifying aerogel.

[0059] It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of protection of the invention. Furthermore, it should be understood that after reading the technical description of this invention, those skilled in the art can make various alterations, modifications, or variations to the invention, and all such equivalent forms also fall 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, weave them into a web, spray adhesive, dry them, and cure them to obtain a lightweight and warm spray-bonded cotton material. 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. 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.

2. 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.

3. 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.

4. 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.

5. 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.

6. 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.

7. A lightweight, heat-insulating spray-bonded cotton material prepared by the preparation method according to any one of claims 1-6.

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