阅读说明：本技术 一种白石墨烯发光再生纤维素纤维及其制备方法 (White graphene luminescent regenerated cellulose fiber and preparation method thereof ) 是由 马立国 沙嫣 沙晓林 于 2021-06-25 设计创作，主要内容包括：本发明公开了一种白石墨烯发光再生纤维素纤维及其制备方法,该方法包含：步骤1,按比例称取各原料；各原料中包含再生纤维素浆粕、白石墨烯微片、发光粉、表面活性剂、碱性试剂；步骤2,制备再生纤维素用纤维素浆粕；步骤3,制备白石墨烯纳米微片；步骤4,将步骤3所得的白石墨烯纳米微片和发光粉加入到步骤2所得的浆粕中充分混合,搅拌,然后将所得的再生纤维素纤维浆粕进行纺丝,制备白石墨烯发光凉感复合长丝纤维。本发明还提供了通过该方法制备的白石墨烯发光再生纤维素纤维。本发明利用白石墨烯微片制备和分散体系,以及改进的再生纤维素纺丝制备得到白石墨烯发光再生纤维素纤维,并使该复合纤维具备抗菌、凉感、发光等功能。(The invention discloses a white graphene luminescent regenerated cellulose fiber and a preparation method thereof, wherein the method comprises the following steps: step 1, weighing raw materials in proportion; each raw material comprises regenerated cellulose pulp, white graphene nanoplatelets, luminescent powder, a surfactant and an alkaline reagent; step 2, preparing cellulose pulp for regenerated cellulose; step 3, preparing white graphene nanoplatelets; and 4, adding the white graphene nanoplatelets and the luminescent powder obtained in the step 3 into the pulp obtained in the step 2, fully mixing, stirring, and spinning the obtained regenerated cellulose fiber pulp to prepare the white graphene luminescent cool composite filament fiber. The invention also provides the white graphene luminescent regenerated cellulose fiber prepared by the method. According to the invention, the white graphene luminescent regenerated cellulose fiber is prepared by utilizing a white graphene microchip preparation and dispersion system and an improved regenerated cellulose spinning, and the composite fiber has the functions of antibiosis, cool feeling, luminescence and the like.)

1. A preparation method of white graphene luminescent regenerated cellulose fibers is characterized by comprising the following steps:

step 1, weighing raw materials in proportion; each raw material comprises regenerated cellulose pulp, white graphene nanoplatelets, luminescent powder, a surfactant and an alkaline reagent;

step 2, preparing cellulose pulp for regenerated cellulose;

step 3, preparing white graphene nanoplatelets;

and 4, adding the white graphene nanoplatelets and the luminescent powder obtained in the step 3 into the pulp obtained in the step 2, fully mixing, stirring, and spinning the obtained regenerated cellulose fiber pulp to prepare the white graphene luminescent cool composite filament fiber.

2. The method for preparing the white graphene luminescent regenerated cellulose fiber according to claim 1, wherein in the step 1, each raw material comprises, by mass, 85% -99% of regenerated cellulose pulp, 0.1% -14% of white graphene nanoplatelets, 0.1% -10% of luminescent powder, 0.1% -5% of surfactant, and 0.1% -1% of alkaline reagent.

3. The method for preparing the white graphene luminescent regenerated cellulose fiber according to claim 2, wherein the alkaline reagent comprises one or more of ammonia water, potassium hydroxide, sodium hydroxide and sodium bicarbonate.

4. The method for preparing the white graphene luminescent regenerated cellulose fiber according to claim 2, wherein the surface activity comprises a mass ratio of 1: (2-3): (3-4): (4-5) polyvinylpyrrolidone, ethyl cellulose, polyvinyl alcohol, and sodium lauryl sulfate.

5. The method for preparing the white graphene luminescent regenerated cellulose fiber according to claim 1, wherein in the step 2, the regenerated cellulose pulp is mixed with a sodium hydroxide solution with the mass fraction of 20-40%, and the mixture is stirred for 20-30min by a stirrer to be completely mixed; putting the mixture into a squeezer for squeezing, wherein the pressure is set to be 1-5 kpa, and the squeezing time is 20-50 min; aging the pulp at 25-30 ℃ for 3-5h, raising the temperature to 35-40 ℃, and aging for 1-2 h; and yellowing is carried out after the aging is finished, wherein the yellowing temperature is 22-25 ℃, the yellowing time is 10-30min, the temperature is increased to 30-35 ℃, and the yellowing time is 40-60 min.

6. The preparation method of the white graphene luminescent regenerated cellulose fiber according to claim 6, wherein the mass ratio of the regenerated cellulose pulp to the sodium hydroxide solution is 1 (2-4).

7. The method for preparing the white graphene luminescent regenerated cellulose fiber according to claim 1, wherein the step 3 comprises:

step 3.1, mixing boron and nitrogen in a mass ratio of 1: (2-4) mixing the boric acid, the urea and the borax by heating to 70-90 ℃, wherein the mass fraction of the borax is 10% -20%, cooling, placing in a vacuum nitriding furnace, heating to 500-;

step 3.2, placing the boron nitride powder in a high-temperature tube furnace, heating to 500-;

and 3.3, immersing the boron nitride nanoplatelets in an alkaline reagent aqueous solution, wherein the mass fraction of the alkaline reagent in the solution is 0.01-0.05%, then heating and mechanically stirring for 3-5h under the condition of oil bath at the temperature of 100-.

8. The method for preparing the white graphene luminescent regenerated cellulose fiber according to claim 1, wherein in the step 4, the white graphene nanoplatelets and the luminescent powder are added into the pulp to be fully mixed, and the mixture is stirred by a stirrer for 10-30 min.

9. The method for preparing the white graphene luminescent regenerated cellulose fiber according to claim 8, wherein in the step 4, the ratio of the solid content of the white graphene to the solid content of the pulp cellulose is (0.01-0.14): 1.

10. a white graphene luminescent regenerated cellulose fiber prepared by the method of any one of claims 1 to 9.

Technical Field

The invention relates to a white graphene luminous cool filament fiber and a preparation method thereof, and particularly relates to a white graphene luminous regenerated cellulose fiber and a preparation method thereof.

Background

"white graphene" is a name given to a nanosheet obtained after exfoliation of Hexagonal Boron Nitride (english name: Hexagonal Boron Nitride, abbreviated as h-BN) with crystal grains in a lamellar structure. Since the structure of hexagonal boron nitride is very similar to that of graphite, it has a hexagonal layered structure, is soft in texture, is highly processable, and is white in color. Corresponding to graphene, hexagonal boron nitride is therefore referred to as "white graphene".

Hexagonal boron nitride and graphene are both layered two-dimensional materials of only one atom thickness, except that graphene is bonded purely by covalent bonds between carbon atoms, whereas the bonds in a hexagonal boron nitride crystal are covalent bonds between boron and nitrogen heterogeneous atoms.

The highly similar crystal structure gives white graphene and graphene some common characteristics, such as extremely high in-plane elastic modulus, high temperature stability, and atomically smooth surface. The white graphene has high transparency and chemical inertness, and has the properties of high mechanical strength, high melting point, high thermal conductivity, extremely low friction coefficient and the like. A monolayer of atomic thick boron nitride can withstand high temperatures of 800 c in air. The white graphene has excellent impermeability, and is very suitable for corrosion prevention of metal under high temperature and corrosive liquid environment. Meanwhile, the latest research of my company discovers that the white graphene also has excellent antibacterial performance and has great development potential in fiber application.

The regenerated cellulose fiber is a cellulose fiber with wide application, has good mechanical property and hygroscopicity, and does not have functionality. The traditional functional regenerated cellulose fiber is mainly realized by adding an auxiliary agent into the regenerated cellulose fiber or modifying the fiber, and the regenerated cellulose fiber prepared by the method has the defects of poor functionality and severe pollution caused by aftertreatment, so that the application of the regenerated cellulose fiber is limited to a certain extent.

Disclosure of Invention

The invention aims to provide a white graphene luminous cool filament fiber and a preparation method thereof, wherein a white graphene microchip preparation and dispersion system and improved regenerated cellulose spinning are utilized to prepare the white graphene luminous regenerated cellulose fiber, and the composite fiber has the functions of antibiosis, cool feeling, luminescence and the like.

In order to achieve the above object, the present invention provides a method for preparing a white graphene luminescent regenerated cellulose fiber, wherein the method comprises: step 1, weighing raw materials in proportion; each raw material comprises regenerated cellulose pulp, white graphene nanoplatelets, luminescent powder, a surfactant and an alkaline reagent; step 2, preparing cellulose pulp for regenerated cellulose; step 3, preparing white graphene nanoplatelets; and 4, adding the white graphene nanoplatelets and the luminescent powder obtained in the step 3 into the pulp obtained in the step 2, fully mixing, stirring, and spinning the obtained regenerated cellulose fiber pulp to prepare the white graphene luminescent cool composite filament fiber.

In the step 1, the raw materials include, by mass, 85% -99% of regenerated cellulose pulp, 0.1% -14% of white graphene nanoplatelets, 0.1% -10% of luminescent powder, 0.1% -5% of surfactant, and 0.1% -1% of alkaline reagent.

The preparation method of the white graphene luminescent regenerated cellulose fiber comprises the step of preparing the white graphene luminescent regenerated cellulose fiber, wherein the alkaline reagent comprises one or more of ammonia water, potassium hydroxide, sodium hydroxide and sodium bicarbonate.

The preparation method of the white graphene luminescent regenerated cellulose fiber comprises the following steps of: (2-3): (3-4): (4-5) polyvinylpyrrolidone, ethyl cellulose, polyvinyl alcohol, and sodium lauryl sulfate.

In the step 2, the regenerated cellulose pulp is mixed with a sodium hydroxide solution with a mass fraction of 20% -40%, and the mixture is stirred for 20-30min by a stirrer to be completely mixed; putting the mixture into a squeezer for squeezing, wherein the pressure is set to be 1-5 kpa, and the squeezing time is 20-50 min; aging the pulp at 25-30 ℃ for 3-5h, raising the temperature to 35-40 ℃, and aging for 1-2 h; and yellowing is carried out after the aging is finished, wherein the yellowing temperature is 22-25 ℃, the yellowing time is 10-30min, the temperature is increased to 30-35 ℃, and the yellowing time is 40-60 min.

The preparation method of the white graphene luminescent regenerated cellulose fiber comprises the step of preparing a white graphene luminescent regenerated cellulose fiber, wherein the mass ratio of the regenerated cellulose pulp to the sodium hydroxide solution is 1 (2-4).

The preparation method of the white graphene luminescent regenerated cellulose fiber comprises the following steps in step 3: step 3.1, mixing boron and nitrogen in a mass ratio of 1: (2-4) mixing the boric acid, the urea and the borax by heating to 70-90 ℃, wherein the mass fraction of the borax is 10% -20%, cooling, placing in a vacuum nitriding furnace, heating to 500-; step 3.2, placing the boron nitride powder in a high-temperature tube furnace, heating to 500-; and 3.3, immersing the boron nitride nanoplatelets in an alkaline reagent aqueous solution, wherein the mass fraction of the alkaline reagent in the solution is 0.01-0.05%, then heating and mechanically stirring for 3-5h under the condition of oil bath at the temperature of 100-.

In the step 4, the white graphene nanoplatelets and the luminescent powder are added into the pulp to be fully mixed, and the mixture is stirred by a stirrer for 10-30 min.

In the preparation method of the white graphene luminescent regenerated cellulose fiber, in the step 4, the ratio of the solid content of the white graphene to the solid content of the pulp cellulose is (0.01-0.14): 1.

the invention also provides the white graphene luminescent regenerated cellulose fiber prepared by the method.

The white graphene luminescent regenerated cellulose fiber and the preparation method thereof provided by the invention have the following advantages:

the white graphene nanoplatelets prepared by the method are thinner, the thickness of the white graphene nanoplatelets is less than 5 nanometers, the thermal conductivity of the white graphene nanoplatelets is better, the white graphene is uniformly distributed in fibers through an optimized dispersion technology, the white graphene nanoplatelets have an excellent heat conduction function, heat generated by a human body can be rapidly dissipated, the surface of the skin of the human body can be rapidly cooled, and the skin of the human body can generate a contact cool feeling. And after a certain amount of white graphene nanoplatelets are added into the regenerated cellulose fibers, more obvious grooves are formed in the fiber spinning process, the capillary wicking effect can be generated, and the two synergistic effects enable the cool feeling of the composite fibers to be more obvious.

The graphene luminescent regenerated cellulose fiber also has excellent antibacterial performance, and tests show that the antibacterial performance of staphylococcus aureus, candida albicans and escherichia coli reaches 99%. Meanwhile, the luminescent powder is added, so that the fibers become gorgeous and colorful, and the additional value of the fibers is improved.

The white graphene luminescent cool composite fiber prepared by the method has the advantages of simple process, easy operation, low cost and high economic benefit, and is suitable for large-scale industrial production.

Detailed Description

The following further describes embodiments of the present invention.

The invention provides a preparation method of white graphene luminescent regenerated cellulose fibers, which comprises the following steps:

step 1, weighing raw materials in proportion; each raw material comprises regenerated cellulose pulp, white graphene nanoplatelets, luminescent powder, a surfactant and an alkaline reagent; step 2, preparing cellulose pulp for regenerated cellulose; step 3, preparing white graphene nanoplatelets; and 4, adding the white graphene nanoplatelets and the luminescent powder obtained in the step 3 into the pulp obtained in the step 2, fully mixing, stirring, and spinning the obtained regenerated cellulose fiber pulp to prepare the white graphene luminescent cool composite filament fiber, namely the white graphene luminescent regenerated cellulose fiber.

Preferably, in the step 1, the raw materials comprise, by mass, 85% -99% of regenerated cellulose pulp, 0.1% -14% of white graphene nanoplatelets, 0.1% -10% of luminescent powder, 0.1% -5% of surfactant and 0.1% -1% of alkaline reagent.

The alkaline reagent comprises any one or more of ammonia water, potassium hydroxide, sodium hydroxide and sodium bicarbonate.

The surface activity comprises the following components in a mass ratio of 1: (2-3): (3-4): (4-5) polyvinylpyrrolidone, ethyl cellulose, polyvinyl alcohol, and sodium lauryl sulfate.

In the step 2, mixing the regenerated cellulose pulp with 20-40% sodium hydroxide solution by mass percent, and stirring for 20-30min by using a stirrer to ensure that the regenerated cellulose pulp and the sodium hydroxide solution are completely mixed; putting the mixture into a squeezer for squeezing, wherein the pressure is set to be 1-5 kpa, and the squeezing time is 20-50 min; aging the pulp at 25-30 ℃ for 3-5h, raising the temperature to 35-40 ℃, and aging for 1-2 h; and yellowing is carried out after the aging is finished, wherein the yellowing temperature is 22-25 ℃, the yellowing time is 10-30min, the temperature is increased to 30-35 ℃, and the yellowing time is 40-60 min.

The mass ratio of the regenerated cellulose pulp to the sodium hydroxide solution is 1 (2-4).

The step 3 comprises the following steps: step 3.1, mixing boron and nitrogen in a mass ratio of 1: (2-4) mixing the boric acid, the urea and the borax by heating to 70-90 ℃, wherein the mass fraction of the borax is 10% -20%, cooling, placing in a vacuum nitriding furnace, heating to 500-; step 3.2, placing the boron nitride powder in a high-temperature tube furnace, heating to 500-; and 3.3, immersing the boron nitride nanoplatelets in an alkaline reagent aqueous solution, wherein the mass fraction of the alkaline reagent in the solution is 0.01-0.05%, then heating and mechanically stirring for 3-5h under the condition of oil bath at the temperature of 100-.

And 4, adding the white graphene nanoplatelets and the luminescent powder into the pulp, fully mixing, and stirring for 10-30min by using a stirrer. The ratio of the solid content of the white graphene to the solid content of the pulp cellulose is (0.01-0.14): 1.

the invention also provides the white graphene luminescent regenerated cellulose fiber prepared by the method.

The following describes the white graphene luminescent regenerated cellulose fiber and the preparation method thereof provided by the present invention with reference to the following embodiments.

Example 1

A preparation method of a white graphene luminescent regenerated cellulose fiber comprises the following steps:

step 1, weighing raw materials in proportion; the raw materials comprise regenerated cellulose pulp, white graphene nanoplatelets, luminescent powder, a surfactant and an alkaline reagent.

Preferably, the raw materials comprise 99% of regenerated cellulose pulp, 0.1% of white graphene nanoplatelets, 0.7% of luminescent powder, 0.1% of surfactant and 0.1% of alkaline reagent by mass percentage.

The alkaline agent comprises ammonia.

The surface activity comprises the following components in a mass ratio of 1: 2: 3: 4, polyvinylpyrrolidone, ethyl cellulose, polyvinyl alcohol and lauryl sodium sulfate.

And 2, preparing cellulose pulp for regenerated cellulose.

Mixing the regenerated cellulose pulp with a sodium hydroxide solution with the mass fraction of 20%, wherein the mass ratio of the regenerated cellulose pulp to the sodium hydroxide solution is 1: 2. Stirring with a stirrer for 20-30min to completely mix; putting the mixture into a squeezer for squeezing, wherein the pressure is set to be 1-5 kpa, and the squeezing time is 20-50 min; aging the pulp at 25-30 ℃ for 3-5h, raising the temperature to 35-40 ℃, and aging for 1-2 h; and yellowing is carried out after the aging is finished, wherein the yellowing temperature is 22-25 ℃, the yellowing time is 10-30min, the temperature is increased to 30-35 ℃, and the yellowing time is 40-60 min.

And 3, preparing the white graphene nanoplatelets.

The step 3 comprises the following steps: step 3.1, mixing boron and nitrogen in a mass ratio of 1:2, mixing the boric acid, the urea and the borax at the mass fraction of 10% under the condition of heating to 70-90 ℃, cooling, placing in a vacuum nitriding furnace, heating to 500-1000 ℃, reacting for 20-50min, heating to 1000-1500 ℃, reacting for 1-2min, cooling, and obtaining the boron nitride powder.

And 3.2, placing the boron nitride powder in a high-temperature tube furnace, heating to 500-800 ℃, cooling, dispersing the powder in distilled water, carrying out ultrasonic stripping treatment for 1-2 hours, and carrying out centrifugal drying to obtain the boron nitride nanoplatelets.

And 3.3, immersing the boron nitride nanosheet in an alkaline reagent aqueous solution, wherein the mass fraction of the alkaline reagent in the solution is 0.01%, then heating and mechanically stirring for 3-5h under the oil bath condition of 100-120 ℃, washing until the filtrate is neutral, and centrifugally drying to obtain the hydroxylated hexagonal boron nitride nanosheet.

And 4, adding the white graphene nanoplatelets and the luminescent powder obtained in the step 3 into the pulp obtained in the step 2, fully mixing, stirring for 10-30min by using a stirrer, wherein the solid content of the white graphene and the solid content of pulp cellulose are (0.01-0.14): 1. and spinning the obtained regenerated cellulose fiber pulp to prepare the white graphene luminous cool composite filament fiber.

The embodiment also provides the white graphene luminescent regenerated cellulose fiber prepared by the method.

Example 2

A preparation method of a white graphene luminescent regenerated cellulose fiber comprises the following steps:

step 1, weighing raw materials in proportion; the raw materials comprise regenerated cellulose pulp, white graphene nanoplatelets, luminescent powder, a surfactant and an alkaline reagent.

Preferably, the raw materials comprise 86% of regenerated cellulose pulp, 2% of white graphene nanoplatelets, 10% of luminescent powder, 1% of surfactant and 1% of alkaline reagent by mass percent.

The alkaline reagent comprises potassium hydroxide.

The surface activity comprises the following components in a mass ratio of 1: 2: 3: 4, polyvinylpyrrolidone, ethyl cellulose, polyvinyl alcohol and lauryl sodium sulfate.

And 2, preparing cellulose pulp for regenerated cellulose.

Mixing the regenerated cellulose pulp with 25% sodium hydroxide solution by mass, wherein the mass ratio of the regenerated cellulose pulp to the sodium hydroxide solution is 1: 2. Stirring with a stirrer for 20-30min to completely mix; putting the mixture into a squeezer for squeezing, wherein the pressure is set to be 1-5 kpa, and the squeezing time is 20-50 min; aging the pulp at 25-30 ℃ for 3-5h, raising the temperature to 35-40 ℃, and aging for 1-2 h; and yellowing is carried out after the aging is finished, wherein the yellowing temperature is 22-25 ℃, the yellowing time is 10-30min, the temperature is increased to 30-35 ℃, and the yellowing time is 40-60 min.

And 3, preparing the white graphene nanoplatelets.

The step 3 comprises the following steps: step 3.1, mixing boron and nitrogen in a mass ratio of 1:2, mixing the boric acid, the urea and the borax under the condition of heating to 70-90 ℃, wherein the mass fraction of the borax is 12%, cooling, placing in a vacuum nitriding furnace, heating to 500-1000 ℃, reacting for 20-50min, heating to 1000-1500 ℃, reacting for 1-2min, cooling, and obtaining the boron nitride powder.

And 3.2, placing the boron nitride powder in a high-temperature tube furnace, heating to 500-800 ℃, cooling, dispersing the powder in distilled water, carrying out ultrasonic stripping treatment for 1-2 hours, and carrying out centrifugal drying to obtain the boron nitride nanoplatelets.

And 3.3, immersing the boron nitride nanosheet in an alkaline reagent aqueous solution, wherein the mass fraction of the alkaline reagent in the solution is 0.02%, then heating and mechanically stirring for 3-5h under the oil bath condition of 100-120 ℃, washing until the filtrate is neutral, and centrifugally drying to obtain the hydroxylated hexagonal boron nitride nanosheet.

And 4, adding the white graphene nanoplatelets and the luminescent powder obtained in the step 3 into the pulp obtained in the step 2, fully mixing, stirring for 10-30min by using a stirrer, wherein the solid content of the white graphene and the solid content of pulp cellulose are (0.01-0.14): 1. and spinning the obtained regenerated cellulose fiber pulp to prepare the white graphene luminous cool composite filament fiber.

The embodiment also provides the white graphene luminescent regenerated cellulose fiber prepared by the method.

Example 3

A preparation method of a white graphene luminescent regenerated cellulose fiber comprises the following steps:

step 1, weighing raw materials in proportion; the raw materials comprise regenerated cellulose pulp, white graphene nanoplatelets, luminescent powder, a surfactant and an alkaline reagent.

Preferably, the raw materials comprise, by mass, 87.2% of regenerated cellulose pulp, 5% of white graphene nanoplatelets, 5% of luminescent powder, 2% of surfactant and 0.8% of alkaline reagent.

The alkaline agent comprises sodium hydroxide.

The surface activity comprises the following components in a mass ratio of 1: 2.5: 3.5: 4.5 of polyvinylpyrrolidone, ethyl cellulose, polyvinyl alcohol and sodium dodecyl sulfate.

And 2, preparing cellulose pulp for regenerated cellulose.

Mixing the regenerated cellulose pulp with a sodium hydroxide solution with the mass fraction of 30%, wherein the mass ratio of the regenerated cellulose pulp to the sodium hydroxide solution is 1: 3. Stirring with a stirrer for 20-30min to completely mix; putting the mixture into a squeezer for squeezing, wherein the pressure is set to be 1-5 kpa, and the squeezing time is 20-50 min; aging the pulp at 25-30 ℃ for 3-5h, raising the temperature to 35-40 ℃, and aging for 1-2 h; and yellowing is carried out after the aging is finished, wherein the yellowing temperature is 22-25 ℃, the yellowing time is 10-30min, the temperature is increased to 30-35 ℃, and the yellowing time is 40-60 min.

And 3, preparing the white graphene nanoplatelets.

The step 3 comprises the following steps: step 3.1, mixing boron and nitrogen in a mass ratio of 1:3, mixing the boric acid, the urea and the borax at the mass fraction of 15% under the condition of heating to 70-90 ℃, cooling, placing in a vacuum nitriding furnace, heating to 500-1000 ℃, reacting for 20-50min, heating to 1000-1500 ℃, reacting for 1-2min, cooling, and obtaining the boron nitride powder.

And 3.2, placing the boron nitride powder in a high-temperature tube furnace, heating to 500-800 ℃, cooling, dispersing the powder in distilled water, carrying out ultrasonic stripping treatment for 1-2 hours, and carrying out centrifugal drying to obtain the boron nitride nanoplatelets.

And 3.3, immersing the boron nitride nanosheet in an alkaline reagent aqueous solution, wherein the mass fraction of the alkaline reagent in the solution is 0.03%, then heating and mechanically stirring for 3-5h under the oil bath condition of 100-120 ℃, washing until the filtrate is neutral, and centrifugally drying to obtain the hydroxylated hexagonal boron nitride nanosheet.

And 4, adding the white graphene nanoplatelets and the luminescent powder obtained in the step 3 into the pulp obtained in the step 2, fully mixing, stirring for 10-30min by using a stirrer, wherein the solid content of the white graphene and the solid content of pulp cellulose are (0.01-0.14): 1. and spinning the obtained regenerated cellulose fiber pulp to prepare the white graphene luminous cool composite filament fiber.

The embodiment also provides the white graphene luminescent regenerated cellulose fiber prepared by the method.

Example 4

A preparation method of a white graphene luminescent regenerated cellulose fiber comprises the following steps:

step 1, weighing raw materials in proportion; the raw materials comprise regenerated cellulose pulp, white graphene nanoplatelets, luminescent powder, a surfactant and an alkaline reagent.

Preferably, the raw materials comprise, by mass, 85.4% of regenerated cellulose pulp, 9% of white graphene nanoplatelets, 0.1% of luminescent powder, 5% of surfactant and 0.5% of alkaline reagent.

The alkaline agent comprises sodium bicarbonate.

The surface activity comprises the following components in a mass ratio of 1: 3: 4: 5, polyvinylpyrrolidone, ethyl cellulose, polyvinyl alcohol and lauryl sodium sulfate.

And 2, preparing cellulose pulp for regenerated cellulose.

Mixing the regenerated cellulose pulp with 35% sodium hydroxide solution by mass, wherein the mass ratio of the regenerated cellulose pulp to the sodium hydroxide solution is 1: 4. Stirring with a stirrer for 20-30min to completely mix; putting the mixture into a squeezer for squeezing, wherein the pressure is set to be 1-5 kpa, and the squeezing time is 20-50 min; aging the pulp at 25-30 ℃ for 3-5h, raising the temperature to 35-40 ℃, and aging for 1-2 h; and yellowing is carried out after the aging is finished, wherein the yellowing temperature is 22-25 ℃, the yellowing time is 10-30min, the temperature is increased to 30-35 ℃, and the yellowing time is 40-60 min.

And 3, preparing the white graphene nanoplatelets.

The step 3 comprises the following steps: step 3.1, mixing boron and nitrogen in a mass ratio of 1:4, mixing the boric acid, the urea and the borax at the mass fraction of 18% under the condition of heating to 70-90 ℃, cooling, placing in a vacuum nitriding furnace, heating to 500-1000 ℃, reacting for 20-50min, heating to 1000-1500 ℃, reacting for 1-2min, cooling, and obtaining the boron nitride powder.

And 3.2, placing the boron nitride powder in a high-temperature tube furnace, heating to 500-800 ℃, cooling, dispersing the powder in distilled water, carrying out ultrasonic stripping treatment for 1-2 hours, and carrying out centrifugal drying to obtain the boron nitride nanoplatelets.

And 3.3, immersing the boron nitride nanosheet in an alkaline reagent aqueous solution, wherein the mass fraction of the alkaline reagent in the solution is 0.04%, then heating and mechanically stirring for 3-5h under the oil bath condition of 100-120 ℃, washing until the filtrate is neutral, and centrifugally drying to obtain the hydroxylated hexagonal boron nitride nanosheet.

And 4, adding the white graphene nanoplatelets and the luminescent powder obtained in the step 3 into the pulp obtained in the step 2, fully mixing, stirring for 10-30min by using a stirrer, wherein the solid content of the white graphene and the solid content of pulp cellulose are (0.01-0.14): 1. and spinning the obtained regenerated cellulose fiber pulp to prepare the white graphene luminous cool composite filament fiber.

The embodiment also provides the white graphene luminescent regenerated cellulose fiber prepared by the method.

Example 5

A preparation method of a white graphene luminescent regenerated cellulose fiber comprises the following steps:

step 1, weighing raw materials in proportion; the raw materials comprise regenerated cellulose pulp, white graphene nanoplatelets, luminescent powder, a surfactant and an alkaline reagent.

Preferably, the raw materials comprise, by mass, 85% of regenerated cellulose pulp, 14% of white graphene nanoplatelets, 0.5% of luminescent powder, 0.3% of surfactant and 0.2% of alkaline reagent.

The alkaline agent comprises any of ammonia, potassium hydroxide, sodium hydroxide, and sodium bicarbonate.

The surface activity comprises the following components in a mass ratio of 1: 3: 4: 5, polyvinylpyrrolidone, ethyl cellulose, polyvinyl alcohol and lauryl sodium sulfate.

And 2, preparing cellulose pulp for regenerated cellulose.

Mixing the regenerated cellulose pulp with a sodium hydroxide solution with the mass fraction of 40%, wherein the mass ratio of the regenerated cellulose pulp to the sodium hydroxide solution is 1: 4. Stirring with a stirrer for 20-30min to completely mix; putting the mixture into a squeezer for squeezing, wherein the pressure is set to be 1-5 kpa, and the squeezing time is 20-50 min; aging the pulp at 25-30 ℃ for 3-5h, raising the temperature to 35-40 ℃, and aging for 1-2 h; and yellowing is carried out after the aging is finished, wherein the yellowing temperature is 22-25 ℃, the yellowing time is 10-30min, the temperature is increased to 30-35 ℃, and the yellowing time is 40-60 min.

And 3, preparing the white graphene nanoplatelets.

The step 3 comprises the following steps: step 3.1, mixing boron and nitrogen in a mass ratio of 1:4, mixing the boric acid, the urea and the borax at the mass fraction of 20% under the condition of heating to 70-90 ℃, cooling, placing in a vacuum nitriding furnace, heating to 500-1000 ℃, reacting for 20-50min, heating to 1000-1500 ℃, reacting for 1-2min, cooling, and obtaining the boron nitride powder.

And 3.2, placing the boron nitride powder in a high-temperature tube furnace, heating to 500-800 ℃, cooling, dispersing the powder in distilled water, carrying out ultrasonic stripping treatment for 1-2 hours, and carrying out centrifugal drying to obtain the boron nitride nanoplatelets.

And 3.3, immersing the boron nitride nanosheet in an alkaline reagent aqueous solution, wherein the mass fraction of the alkaline reagent in the solution is 0.05%, then heating and mechanically stirring for 3-5h under the oil bath condition of 100-120 ℃, washing until the filtrate is neutral, and centrifugally drying to obtain the hydroxylated hexagonal boron nitride nanosheet.

And 4, adding the white graphene nanoplatelets and the luminescent powder obtained in the step 3 into the pulp obtained in the step 2, fully mixing, stirring for 10-30min by using a stirrer, wherein the solid content of the white graphene and the solid content of pulp cellulose are (0.01-0.14): 1. and spinning the obtained regenerated cellulose fiber pulp to prepare the white graphene luminous cool composite filament fiber.

The embodiment also provides the white graphene luminescent regenerated cellulose fiber prepared by the method.

And testing the finished product obtained in each embodiment, wherein the brightness test is carried out on the white graphene luminescent fiber by adopting a brightness meter, the fabric cool feeling is tested by adopting standard FTTS-FA-019, and the fiber proportion is screened and optimized. The results are shown in table 1 below.

TABLE 1 test results.

The invention provides a white graphene luminescent regenerated cellulose fiber and a preparation method thereof. The white graphene nanometer microchip with thinner particle size is newly introduced into the formula, and the aim is to prepare a white graphene luminous cool filament fiber by utilizing a white graphene microchip preparation and dispersion system and improved regenerated cellulose spinning, so that the composite fiber has the functions of antibiosis, cool feeling, luminescence and the like. The composite fiber has excellent antibacterial performance, and tests show that the antibacterial performance of staphylococcus aureus, candida albicans and escherichia coli reaches 99%. Meanwhile, the luminescent powder is added, so that the fibers become gorgeous and colorful, and the additional value of the fibers can be improved.

While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention. Various modifications and alterations to this invention will become apparent to those skilled in the art upon reading the foregoing description. Accordingly, the scope of the invention should be determined from the following claims.