Soft warm-keeping polyester wadding material and preparation method thereof

Abstract

The invention relates to the technical field of fabric spinning, and discloses a soft warm-keeping polyester wadding material and a preparation method thereof. Silk fibroin, phloroglucinol triglycidyl ether and graphene are combined and added into a polyester material, and the thin, soft and warm-keeping polyester wadding material is obtained. The phloroglucinol triglycidyl ether can be bridged with the graphene, the silk fibroin and the polyester fiber, the uniformly dispersed graphene sheet layers construct a continuous and efficient three-dimensional conductive network path in the polyester fiber through mutual contact and lap joint and a quantum tunneling effect, the volume resistivity and the surface resistivity of the fiber are remarkably reduced, and the conductivity of the fiber is improved. Accumulated static charges can be quickly discharged, and the antistatic property of the material is improved; and the phloroglucinol triglycidyl ether contains a benzene ring which forms pi-pi interaction with the polyester, so that the compatibility of the silk fibroin and the polyester is improved, and the properties of thermal insulation and the like of the polyester wadding are improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of fabric spinning, in particular to a light and soft 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, which has the characteristics of high bulkiness, lightness, softness, etc. In the traditional process, the fiber raw material is carded into a single layer of thin net, and then is laid into a flake, and the intersection points between the fibers are bonded by spraying adhesive on both sides of the flake, and then are dried and solidified. Because the contact intersection points of the material are more and the bridging points are less, the material has the characteristics of softness, softness and elasticity. In recent years, spray glue cotton has been widely used in all aspects of people's life, and has become one of the main raw materials for processing and manufacturing cotton clothes, home clothes, cotton quilts or sleeping bags, even industrial products.

[0003] The most widely used spray glue cotton raw material fiber at present 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. But the polyester fiber has no hydrophilic gene in the internal macromolecule, so the moisture absorption and moisture permeability are low, the comfort of the clothes made of it is poor, and it will produce odor after long-term use. Silk fibroin contains a large number of hydrophilic chemical groups such as hydroxyl, amide and oxygen groups. The introduction of these groups into synthetic fibers can improve the defect of poor moisture absorption, increase the moisture regain of the fibers, and further improve the comfort of the clothes, which is beneficial to improve the strength of the fibers, but the compatibility between the polyester fibers is poor, and the intermediate substance is needed to connect; the longitudinal and transverse of graphene modified fiber exist some small holes, and the surface is inlaid with dense graphene particles. The structure makes the specific surface area of the fiber increase, which is more conducive to the contact with sweat, so as to absorb moisture and generate heat. The unique porous structure of the fiber makes the woven fabric fluffy and light, which is beneficial to store air and reduce heat exchange, and has the effect of heat storage and temperature rise. SUMMARY

[0004] (I) Technical problems to be solved:

[0005] In view of the shortcomings of the prior art, the present application provides a light and soft warm spray glue cotton material and a preparation method thereof, which solves the problems of poor warm keeping, poor moisture absorption, poor antistatic performance and the like of the traditional spray glue cotton material.

[0006] (II) Technical scheme: The preparation method of the light and soft warm spray glue cotton material comprises the following steps:

[0007] Step (1), adding graphene oxide to water, ultrasonic dispersion, then adding m-phenol triol triglycidyl ether and silk fibroin into a beaker, stirring and reacting, and freeze-drying to remove water to obtain silk fibroin crosslinked grafted graphene.

[0008] Step (2), polyethylene terephthalate, silk fibroin crosslinking grafting graphene is extruded in a screw extruder, pelletized, and then melt spun in a melt spinning machine, drawn, to obtain a graphene polyester fiber.

[0009] Step (3), the graphene polyester fiber is sprayed with an adhesive, dried and cured to obtain a light and soft warm sprayed cotton material.

[0010] Further, in step (1), the amount of graphene is 100 parts by weight, the amount of resorcinol triglycidyl ether is 30-70 parts by weight, and the amount of silk fibroin is 400-1200 parts by weight.

[0011] Further, in step (1), the stirring reaction time is 6-12h, the stirring reaction temperature is 40-60℃, and the stirring speed is 300-800rpm.

[0012] Further, in step (2), the amount of polyethylene terephthalate is 100 parts by weight, and the amount of silk fibroin crosslinking grafting graphene is 2-25 parts by weight.

[0013] Further, in step (2), 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 (2), 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 adhesive is an acrylic adhesive.

[0016] Further, in step (3), the curing temperature is 80-100℃, and the curing time is 8-15min.

[0017] (III) Beneficial technical effects:

[0018] The silk fibroin is combined with resorcinol triglycidyl ether and graphene and added into polyester material. The resorcinol triglycidyl ether has three epoxy groups, which can bridge graphene and silk fibroin and polyester fiber, successfully introduce hydrophilic groups into the fiber, reduce the frequency of static electricity of the sprayed cotton due to charge accumulation, and improve the antistatic property. Moreover, the resorcinol triglycidyl ether contains benzene rings, which form π-π interaction with polyester, improving the compatibility of silk fibroin and polyester, which is beneficial to improve the warmth retention performance of the sprayed cotton. At the same time, graphene exhibits good compatibility with the polyester matrix due to its unique two-dimensional sheet structure and surface properties, and can be highly uniformly dispersed in the polyester matrix. The uniformly dispersed graphene sheets form a continuous and efficient three-dimensional conductive network path inside the polyester fiber through mutual contact and quantum tunneling effect, which significantly reduces the volume resistivity and surface resistivity of the fiber, allowing the accumulated static charge to be quickly discharged, thereby endowing the polyester fiber with excellent and durable antistatic properties. DETAILED DESCRIPTION

[0019] In order to make the purpose, technical scheme and advantages of the embodiments of the present application more clear, the technical scheme in the embodiments of the present application will be clearly and completely described below. If the specific conditions are not specified in the embodiments, the conventional conditions or the conditions recommended by the manufacturer 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.

[0020] Embodiment 1:

[0021] (1) 20 g of graphene oxide was added to water, and after ultrasonic dispersion, 6 g of resorcinol triglycidyl ether and 240 g of silk fibroin were added into a beaker, stirred at 40℃ for 12 h at a speed of 300 rpm, and then freeze-dried to remove water to obtain silk fibroin crosslinked grafted graphene.

[0022] (2) 1000 g of polyethylene terephthalate and 20 g of silk fibroin crosslinked grafted graphene were extruded in a screw extruder, the temperature of 1-5 zone was 240℃, 250℃, 260℃, 265℃, 265℃, and the granulation was carried out at a screw speed of 50 r / min, and then melt spinning was carried out at 300℃ at a speed of 600 m / min in a melt spinning machine, the temperature of 1-4 zone was 285℃, 295℃, 295℃, 300℃, and then drawing was carried out after spinning at a draw ratio of 3.5 times to obtain graphene polyester fiber.

[0023] (3) The graphene polyester fiber was sprayed with acrylic resin adhesive and dried and cured at 100℃ for 8 min to obtain a light and soft warm sprayed cotton material.

[0024] Embodiment 2:

[0025] (1), 20 g graphene oxide was added to water, after ultrasonic dispersion, 8 g phloroglucinol triglycidyl ether, 100 g silk fibroin were put into a beaker, stirred at 50℃ for 8 h, the rotation speed was 500 rpm, freeze-drying to remove water, to obtain silk fibroin crosslinked grafted graphene.

[0026] (2), 1000 g polyethylene terephthalate, 100 g silk fibroin crosslinked grafted graphene were extruded in a screw extruder, the temperature of 1-5 zone was 240℃, 250℃, 260℃, 265℃, 265℃, pelletizing, the screw rotation speed was 70 r / min, melt spinning in a melt spinning machine at a speed of 800 m / min, the temperature of 1-4 zone was 285℃, 295℃, 295℃, 300℃, after spinning, drawing was carried out, the multiple was 3 times, to obtain graphene polyester fiber.

[0027] (3), the graphene polyester fiber was sprayed with acrylic resin adhesive, dried and cured at 90℃ for 12 min, to obtain light and soft warm spray glue cotton material.

[0028] Example 3:

[0029] (1), 20 g graphene oxide was added to water, after ultrasonic dispersion, 14 g phloroglucinol triglycidyl ether, 80 g silk fibroin were put into a beaker, stirred at 60℃ for 6 h, the rotation speed was 800 rpm, freeze-drying to remove water, to obtain silk fibroin crosslinked grafted graphene.

[0030] (2), 1000 g polyethylene terephthalate, 180 g silk fibroin crosslinked grafted graphene were extruded in a screw extruder, the temperature of 1-5 zone was 240℃, 250℃, 260℃, 265℃, 265℃, pelletizing, the screw rotation speed was 120 r / min, then melt spinning in a melt spinning machine at a speed of 1000 m / min at 285℃, the temperature of 1-4 zone was 285℃, 295℃, 295℃, 300℃, after spinning, drawing was carried out, the multiple was 3 times, to obtain graphene polyester fiber.

[0031] (3), the graphene polyester fiber was sprayed with acrylic resin adhesive, dried and cured at 100℃ for 13 min, to obtain light and soft warm spray glue cotton material.

[0032] Example 4:

[0033] (1), 20 g graphene oxide was added to water, after ultrasonic dispersion, 12 g phloroglucinol triglycidyl ether, 220 g silk fibroin were put into a beaker, stirred at 55℃ for 10 h, the rotation speed was 600 rpm, freeze-drying to remove water, to obtain silk fibroin crosslinked grafted graphene.

[0034] (2), 1000 g of polyethylene terephthalate, 250 g of silk fibroin crosslinked grafted graphene were extruded in a screw extruder, the temperature of 1-5 zone was 240℃, 250℃, 260℃, 265℃, 265℃, pelletizing, the screw speed was 90 r / min, then melt spinning at 295℃ in a melt spinning machine at a speed of 700 m / min, the temperature of 1-4 zone was 285℃, 295℃, 295℃, 300℃, drawing was carried out after spinning, the draw ratio was 3.5 times, to obtain graphene polyester fiber.

[0035] (3), the graphene polyester fiber was sprayed with acrylic resin adhesive, dried and cured at 80℃ for 15 min, to obtain a light and soft warm spray glue cotton material.

[0036] Comparative Example 1:

[0037] (1), 20 g of graphene oxide was added to water, after ultrasonic dispersion, 240 g of silk fibroin was added, stirring at 40℃ for 12 h, the speed was 300 rpm, freeze-drying to remove water, to obtain silk fibroin-graphene.

[0038] (2), 1000 g of polyethylene terephthalate, 20 g of silk fibroin-graphene were extruded in a screw extruder, the temperature of 1-5 zone was 240℃, 250℃, 260℃, 265℃, 265℃, pelletizing, the screw speed was 50 r / min, then melt spinning at 300℃ in a melt spinning machine at a speed of 600 m / min, the temperature of 1-4 zone was 285℃, 295℃, 295℃, 300℃, drawing was carried out after spinning, the draw ratio was 3.5 times, to obtain graphene polyester fiber.

[0039] (3), the graphene polyester fiber was sprayed with acrylic resin adhesive, dried and cured at 100℃ for 8 min, to obtain a spray glue cotton material.

[0040] Comparative Example 2:

[0041] (1), 20 g of graphene oxide was added to water, after ultrasonic dispersion, 6 g of ethylene glycol diglycidyl ether, 240 g of silk fibroin was added into a beaker, stirring at 40℃ for 12 h, the speed was 300 rpm, freeze-drying to remove water, to obtain silk fibroin crosslinked grafted graphene.

[0042] (2), 1000 g of polyethylene terephthalate, 20 g of silk fibroin crosslinked grafted graphene are extruded in a screw extruder, the temperature of 1-5 zones is 240℃, 250℃, 260℃, 265℃, 265℃, granulation, the screw speed is 50 r / min, then melt spinning at 300℃ in a melt spinning machine at a speed of 600 m / min, the temperature of 1-4 zones is 285℃, 295℃, 295℃, 300℃, drawing after spinning, the draw ratio is 3.5 times, to obtain graphene polyester fiber.

[0043] (3), the graphene polyester fiber is sprayed with acrylic resin adhesive, dried and cured at 100℃ for 8 min to obtain a sprayed cotton material.

[0044] Moisture absorption test:

[0045] The sprayed cotton material is placed in a constant temperature and humidity chamber (temperature 25℃, humidity 65%) for 48 h and weighed, recorded as W1. Then the sample is transferred to an oven and baked at 110℃ until constant weight, recorded as W2. The moisture regain is calculated according to the formula: moisture regain (%) = (W1-W2) / W2 x 100%.

[0046] Static performance test: tested according to the method specified in the standard FZ / T 01042-1996.

[0047] Thermal insulation performance test: tested according to GB / T 11048-2008 "Textiles-Determination of thermal and water vapour resistance under steady-state conditions (evaporimeter method)".

[0048] Table 1 Performance of sprayed cotton material

[0049]

[0050] In examples 1-4, silk fibroin is combined with resorcinol triglycidyl ether and graphene and added to polyester material. Resorcinol triglycidyl ether has three epoxy groups, which can bridge graphene and silk fibroin and polyester fiber, successfully introducing hydrophilic groups into the fiber, reducing the frequency of static electricity caused by charge accumulation in the sprayed cotton, and improving the antistatic property. In addition, resorcinol triglycidyl ether contains a benzene ring, which forms a π-π interaction with polyester, improving the compatibility of silk fibroin and polyester, which is beneficial to improving the warmth retention performance of the sprayed cotton. At the same time, graphene exhibits good compatibility with the polyester matrix due to its unique two-dimensional sheet structure and surface properties, enabling highly uniform dispersion in the polyester matrix. The uniformly dispersed graphene sheets form a continuous and efficient three-dimensional conductive network path inside the polyester fiber through mutual contact and quantum tunneling effect, which significantly reduces the volume resistivity and surface resistivity of the fiber, allowing the accumulated static charge to be quickly discharged, thereby endowing the polyester fiber with excellent and durable antistatic properties.

[0051] The graphene and silk fibroin of Comparative Example 1 are in a physical blending state, and the compatibility of the two with the polyester fiber is poor, and the dispersibility in the spray glue cotton is low, resulting in poor hydrophilic moisture absorption, antistatic performance and warm-keeping performance of the spray glue cotton.

[0052] Comparative Example 2 utilizes conventional ethylene glycol diglycidyl ether to perform crosslinking reaction on graphene oxide and silk fibroin, and the ethylene glycol diglycidyl ether does not contain a benzene ring, and it is difficult to form π-π bond interaction with the polyester fiber, resulting in low compatibility of the silk fibroin grafted graphene with the polyester fiber, and poor dispersibility in the spray glue cotton, resulting in lower hydrophilic moisture absorption, antistatic performance and warm-keeping performance of the spray glue cotton than Example 1.

[0053] It should be understood that the use of these examples is only for the purpose of illustrating the present application and is not intended to limit the scope of protection of the present application. In addition, it should also be understood that after reading the technical content of the present application, those skilled in the art can make various modifications, modifications or variations to the present application, and all these equivalent forms also fall within the scope of protection defined by the claims attached hereto.

Claims

1. A method for preparing a soft and warm spray-bonded cotton material, characterized in that, The preparation method comprises the following steps: Step (1): Add graphene oxide to water, disperse it by ultrasonication, add phloroglucinol triglycidyl ether and silk fibroin to a beaker, stir to react, freeze dry to remove water, and obtain silk fibroin cross-linked grafted graphene. Step (2): Polyethylene terephthalate and silk fibroin cross-grafted graphene are extruded and pelletized in a screw extruder, then melt-spun and drawn in a melt spinning machine to obtain graphene polyester fiber. Step (3): Spray the graphene polyester fiber with adhesive, dry and cure to obtain a soft and warm spray-bonded cotton material.

2. The method for preparing the soft and warm spray-bonded cotton material according to claim 1, characterized in that, In step (1), the amount of graphene used is 100 parts by weight, the amount of phloroglucinol triglycidyl ether used is 30-70 parts by weight, and the amount of silk fibroin used is 400-1200 parts by weight.

3. The method for preparing the soft and warm spray-bonded cotton material according to claim 1, characterized in that, In step (1), the stirring reaction time is 6-12 hours, the stirring reaction temperature is 40-60℃, and the stirring speed is 300-800 rpm.

4. The method for preparing the soft and warm spray-bonded cotton material according to claim 1, characterized in that, In step (2), the amount of polyethylene terephthalate is 100 parts by weight, and the amount of silk fibroin cross-linked grafted graphene is 2-25 parts by weight.

5. The method for preparing the soft and warm spray-bonded cotton material according to claim 1, characterized in that, In step (2), the temperature of zones 1-5 of the screw extruder is 240-265℃, and the screw speed is 50-120r / min.

6. The method for preparing the soft and warm spray-bonded cotton material according to claim 1, characterized in that, In step (2), 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.

7. The method for preparing the soft and warm spray-bonded cotton material according to claim 1, characterized in that, In step (3), the adhesive is an acrylic resin adhesive.

8. The method for preparing the soft and warm 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 soft and warm spray-bonded cotton material obtained by the preparation method according to any one of claims 1-8.

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