阅读说明：本技术 一种白石墨烯凉感复合纤维及其制备方法 (White graphene cool composite fiber and preparation method thereof ) 是由 李栋 沙嫣 沙晓林 马立国 于 2021-08-31 设计创作，主要内容包括：本发明公开了一种白石墨烯凉感复合纤维及其制备方法,该方法包含：步骤1,按比例称取各原料；步骤2,将再生纤维素浆粕与碱性助剂的水溶液混合,搅拌均匀后放入压榨机中压榨；然后将浆粕进行老成处理；老成完成后再进行黄化；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加入到步骤2所得的浆粕中充分混合,搅拌,然后将制备的白石墨烯再生纤维素纤维浆粕进行纺丝,制备白石墨烯凉感复合长丝纤维。本发明还提供了通过该方法制备的白石墨烯凉感复合纤维。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一种白石墨烯凉感复合长丝纤维,使该复合纤维具备抗菌、凉感等功能。(The invention discloses a white graphene cool composite fiber and a preparation method thereof, wherein the method comprises the following steps: step 1, weighing raw materials in proportion; step 2, mixing the regenerated cellulose pulp with an aqueous solution of an alkaline assistant, uniformly stirring, and then putting into a squeezer for squeezing; then carrying out aging treatment on the pulp; yellowing is carried out after the aging is finished; step 3, preparing white graphene nanoplatelets; and 4, adding the white graphene nanoplatelets obtained in the step 3 into the pulp obtained in the step 2, fully mixing, stirring, and spinning the prepared white graphene regenerated cellulose fiber pulp to prepare the white graphene cool composite filament fiber. The invention also provides the white graphene cool composite fiber prepared by the method. According to the invention, the white graphene cool composite filament fiber is prepared by utilizing a white graphene microchip preparation and dispersion system and an improved regenerated cellulose spinning, so that the composite fiber has the functions of antibiosis, cool feeling and the like.)

1. A preparation method of white graphene cool composite fibers is characterized by comprising the following steps:

step 1, weighing raw materials in proportion;

step 2, mixing the regenerated cellulose pulp with an aqueous solution of an alkaline assistant, uniformly stirring, and then putting into a squeezer for squeezing; then carrying out aging treatment on the pulp; yellowing is carried out after the aging is finished;

step 3, preparing white graphene nanoplatelets;

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

2. The method for preparing the white graphene cool-feeling composite 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, 0.1% -5% of a modifier, and 0.1% -1% of an alkaline assistant.

3. The method for preparing the white graphene cool composite fiber according to claim 2, wherein the alkaline auxiliary agent comprises one or more of ammonia water, potassium hydroxide, sodium hydroxide and sodium bicarbonate.

4. The method for preparing the white graphene cool composite fiber according to claim 2, wherein the modifier is a surfactant and comprises polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone and sodium dodecyl sulfate.

5. The preparation method of the white graphene cool composite fiber according to claim 4, wherein in the surfactant, polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone and sodium dodecyl sulfate are mixed according to a mass ratio of 1: (1-2): (2-4): (3-5) mixing.

6. The preparation method of the white graphene cool-feeling composite fiber according to claim 1, wherein in the step 2, the regenerated cellulose pulp is mixed with the aqueous solution of the alkaline assistant according to the mass ratio of 1 (2-4), the mixture is stirred by a stirrer for 20-30min to be completely and uniformly mixed, and then the mixture is placed into a squeezer to be squeezed, 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 10-30 min, the temperature is increased to 30-35 ℃, and the yellowing time is 40-60 min.

7. The method for preparing the white graphene cool composite fiber according to claim 6, wherein the mass fraction of the aqueous solution of the alkaline assistant is 20-40%.

8. The method for preparing the white graphene cool composite fiber according to claim 1, wherein the step 3 comprises:

step 3.1, mixing boric acid, urea and borax under a heating condition, cooling, placing in a vacuum nitriding furnace, heating for reaction, cooling, and cooling to obtain boron nitride powder;

step 3.2, placing the boron nitride powder in a high-temperature tube furnace, heating, cooling, dispersing the powder in distilled water, performing ultrasonic stripping treatment, and performing centrifugal drying to obtain boron nitride nanoplatelets;

and 3.3, placing the boron nitride nanoplatelets in an aqueous solution of an alkaline assistant, heating and mechanically stirring under the condition of oil bath, then washing until the filtrate is neutral, and centrifugally drying to obtain the hydroxylated hexagonal boron nitride nanoplatelets.

9. The method for preparing the white graphene cool composite fiber according to claim 8, wherein in the step 3.1, the mass ratio of boron to nitrogen is 1: (2-4) 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 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 500-800 ℃, cooling, dispersing the powder in distilled water, carrying out ultrasonic stripping treatment for 1-2 hours, and carrying out centrifugal drying to obtain boron nitride nanoplatelets; and 3.3, placing the boron nitride nanosheets in an alkaline solution, 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 nanosheets.

10. A white graphene cool-feeling composite fiber prepared by the method according to any one of claims 1 to 9.

Technical Field

The invention relates to a white graphene composite fiber in the technical field of novel functional polymer materials and a preparation method thereof, and particularly relates to a white graphene cool feeling composite 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 composite fiber and a preparation method thereof, and aims to prepare a white graphene cool composite 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 and the like.

In order to achieve the above object, the present invention provides a method for preparing a white graphene cool composite fiber, wherein the method comprises: step 1, weighing raw materials in proportion; step 2, mixing the regenerated cellulose pulp with an aqueous solution of an alkaline assistant, uniformly stirring, and then putting into a squeezer for squeezing; then carrying out aging treatment on the pulp; yellowing is carried out after the aging is finished; step 3, preparing white graphene nanoplatelets; and 4, adding the white graphene nanoplatelets obtained in the step 3 into the pulp obtained in the step 2, fully mixing, stirring, and spinning the prepared white graphene regenerated cellulose fiber pulp to prepare the white graphene 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, 0.1% -5% of a modifier, and 0.1% -1% of an alkaline assistant.

The preparation method of the white graphene cool composite fiber comprises the step of preparing the white graphene cool composite fiber, wherein the alkaline auxiliary agent comprises one or more of ammonia water, potassium hydroxide, sodium hydroxide and sodium bicarbonate.

The preparation method of the white graphene cool composite fiber comprises the step of preparing a white graphene cool composite fiber, wherein the modifier is a surfactant and comprises polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone and sodium dodecyl sulfate.

The preparation method of the white graphene cool composite fiber comprises the following steps of, in the surfactant, mixing polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone and sodium dodecyl sulfate according to a mass ratio of 1: (1-2): (2-4): (3-5) mixing.

In the step 2, the regenerated cellulose pulp is mixed with the aqueous solution of the alkaline assistant according to the mass ratio of 1 (2-4), the mixture is stirred by a stirrer for 20-30min, and the mixture is placed into a squeezer to be squeezed after being completely and uniformly mixed, 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 10-30 min, the temperature is increased to 30-35 ℃, and the yellowing time is 40-60 min.

The preparation method of the white graphene cool composite fiber comprises the step of preparing the aqueous solution of the alkaline assistant by using a solvent, wherein the mass fraction of the aqueous solution of the alkaline assistant is 20-40%.

The preparation method of the white graphene cool composite fiber comprises the following steps in step 3: step 3.1, mixing boric acid, urea and borax under a heating condition, cooling, placing in a vacuum nitriding furnace, heating for reaction, cooling, and cooling to obtain boron nitride powder; step 3.2, placing the boron nitride powder in a high-temperature tube furnace, heating, cooling, dispersing the powder in distilled water, performing ultrasonic stripping treatment, and performing centrifugal drying to obtain boron nitride nanoplatelets; and 3.3, placing the boron nitride nanoplatelets in an aqueous solution of an alkaline assistant, heating and mechanically stirring under the condition of oil bath, then washing until the filtrate is neutral, and centrifugally drying to obtain the hydroxylated hexagonal boron nitride nanoplatelets.

The preparation method of the white graphene cool composite fiber comprises the following steps of, in step 3.1, mixing boron and nitrogen in a mass ratio of 1: (2-4) 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 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 500-800 ℃, cooling, dispersing the powder in distilled water, carrying out ultrasonic stripping treatment for 1-2 hours, and carrying out centrifugal drying to obtain boron nitride nanoplatelets; and 3.3, placing the boron nitride nanosheets in an alkaline solution, 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 nanosheets.

The invention also provides the white graphene cool composite fiber prepared by the method.

The white graphene cool composite fiber and the preparation method thereof provided by the invention have the following advantages:

according to the invention, a thinner white graphene nano microchip is newly introduced into the formula, the prepared white graphene nano microchip is thinner, the thickness is less than 5 nanometers, the thermal conductivity is better, the white graphene is uniformly distributed in the fiber through an optimized dispersion technology, the white graphene nano microchip has an excellent thermal conductivity function, the heat generated by a human body can be rapidly dissipated, the rapid cooling of the surface of the skin of the human body is realized, and the skin of the human body is enabled to 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. Meanwhile, the white graphene cool composite cellulose fiber also has excellent antibacterial performance, and tests show that the antibacterial performance of staphylococcus aureus, candida albicans and escherichia coli reaches 99%.

The white graphene 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 cool composite fiber, which comprises the following steps:

step 1, weighing raw materials in proportion; step 2, mixing the regenerated cellulose pulp with an aqueous solution of an alkaline assistant, uniformly stirring, and then putting into a squeezer for squeezing; then carrying out aging treatment on the pulp; yellowing is carried out after the aging is finished; step 3, preparing white graphene nanoplatelets; and 4, adding the white graphene nanoplatelets obtained in the step 3 into the pulp obtained in the step 2, fully mixing, stirring, and spinning the prepared white graphene regenerated cellulose fiber pulp to prepare the white graphene cool composite filament fiber.

Preferably, in the step 1, the raw materials comprise, by mass, 85% -99% of regenerated cellulose pulp, 0.1% -14% of white graphene, 0.1% -5% of a modifier, and 0.1% -1% of an alkaline assistant.

The alkaline assistant comprises one or more of ammonia water, potassium hydroxide, sodium bicarbonate and the like.

The modifier is surfactant containing polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone (PVP) and sodium dodecyl sulfate.

In the surfactant, polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone and sodium dodecyl sulfate are mixed according to the mass ratio of 1: (1-2): (2-4): (3-5) mixing.

In the step 2, mixing the regenerated cellulose pulp with an aqueous solution of an alkaline assistant according to a mass ratio of 1 (2-4), stirring for 20-30min by a stirrer, putting the mixture into a squeezer for squeezing after the mixture is completely and uniformly mixed, and setting the pressure to be 1-5 kpa and the squeezing time to be 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 10-30 min, the temperature is increased to 30-35 ℃, and the yellowing time is 40-60 min.

The mass fraction of the aqueous solution of the alkaline auxiliary agent is 20-40%.

The step 3 comprises the following steps: step 3.1, mixing boric acid, urea and borax under a heating condition, cooling, placing in a vacuum nitriding furnace, heating for reaction, cooling, and cooling to obtain boron nitride powder; step 3.2, placing the boron nitride powder in a high-temperature tube furnace, heating, cooling, dispersing the powder in distilled water, performing ultrasonic stripping treatment, and performing centrifugal drying to obtain boron nitride nanoplatelets; and 3.3, placing the boron nitride nanoplatelets in an aqueous solution of an alkaline assistant, heating and mechanically stirring under the condition of oil bath, then washing until the filtrate is neutral, and centrifugally drying to obtain the hydroxylated hexagonal boron nitride nanoplatelets.

In step 3.1, the mass ratio of boron to nitrogen is 1: (2-4) 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 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 500-800 ℃, cooling, dispersing the powder in distilled water, carrying out ultrasonic stripping treatment for 1-2 hours, and carrying out centrifugal drying to obtain boron nitride nanoplatelets; in step 3.3, the boron nitride nanoplatelets are placed in an alkaline solution, wherein the alkaline solution can be a sodium hydroxide aqueous solution with the mass fraction of 20-40%. 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 nanosheets.

The invention also provides the white graphene cool composite fiber prepared by the method.

The white graphene cool composite fiber and the preparation method thereof provided by the invention are further described with reference to the following examples.

Example 1

A preparation method of a white graphene cool composite fiber comprises the following steps:

step 1, weighing the raw materials in proportion.

Preferably, each raw material comprises 99% of regenerated cellulose pulp, 0.1% of white graphene, 0.8% of modifier and 0.1% of alkaline assistant by mass percentage.

The basic auxiliary agent comprises ammonia water.

The modifier adopts a surfactant, comprises polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone and sodium dodecyl sulfate, and is prepared from the following raw materials in a mass ratio of 1: 1: 2: 3, mixing.

Step 2, mixing the regenerated cellulose pulp with an aqueous solution of an alkaline assistant according to the mass ratio of 1:2, wherein the mass fraction of the aqueous solution of the alkaline assistant is 20%; stirring for 20-30min by a stirrer, completely and uniformly mixing, and then putting into a squeezer for squeezing, wherein the set pressure is 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 10-30 min, 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, placing the boron nitride nanosheets in an alkaline solution, 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 nanosheets.

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

The embodiment also provides the white graphene cool composite fiber prepared by the method.

Example 2

A preparation method of a white graphene cool composite fiber comprises the following steps:

step 1, weighing the raw materials in proportion.

Preferably, each raw material comprises, by mass, 94.5% of regenerated cellulose pulp, 4% of white graphene, 1% of a modifier and 0.5% of an alkaline assistant.

The alkaline builder comprises potassium hydroxide.

The modifier adopts a surfactant, comprises polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone and sodium dodecyl sulfate, and is prepared from the following raw materials in a mass ratio of 1: 1.3: 2.5: 3.5 mixing.

Step 2, mixing the regenerated cellulose pulp with an aqueous solution of an alkaline assistant according to the mass ratio of 1:2.5, wherein the mass fraction of the aqueous solution of the alkaline assistant is 25%; stirring for 20-30min by a stirrer, completely and uniformly mixing, and then putting into a squeezer for squeezing, wherein the set pressure is 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 10-30 min, 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 1:2.5, 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, placing the boron nitride nanosheets in an alkaline solution, 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 nanosheets.

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

The embodiment also provides the white graphene cool composite fiber prepared by the method.

Example 3

A preparation method of a white graphene cool composite fiber comprises the following steps:

step 1, weighing the raw materials in proportion.

Preferably, each raw material comprises 86% of regenerated cellulose pulp, 8% of white graphene, 5% of a modifier and 1% of an alkaline assistant by mass percentage.

The alkaline builder comprises sodium hydroxide.

The modifier adopts a surfactant, comprises polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone and sodium dodecyl sulfate, and is prepared from the following raw materials in a mass ratio of 1: 1.5: 3: 4, mixing.

Step 2, mixing the regenerated cellulose pulp with an aqueous solution of an alkaline assistant according to the mass ratio of 1:3, wherein the mass fraction of the aqueous solution of the alkaline assistant is 30%; stirring for 20-30min by a stirrer, completely and uniformly mixing, and then putting into a squeezer for squeezing, wherein the set pressure is 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 10-30 min, 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, placing the boron nitride nanosheets in an alkaline solution, 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 nanosheets.

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

The embodiment also provides the white graphene cool composite fiber prepared by the method.

Example 4

A preparation method of a white graphene cool composite fiber comprises the following steps:

step 1, weighing the raw materials in proportion.

Preferably, each raw material comprises 86.5% of regenerated cellulose pulp, 10% of white graphene, 3% of modifier and 0.3% of alkaline assistant in percentage by mass.

The alkaline builder comprises sodium bicarbonate.

The modifier adopts a surfactant, comprises polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone and sodium dodecyl sulfate, and is prepared from the following raw materials in a mass ratio of 1: 1.8: 3.5: 4.5 mixing.

Step 2, mixing the regenerated cellulose pulp with an aqueous solution of an alkaline assistant according to the mass ratio of 1:3.5, wherein the mass fraction of the aqueous solution of the alkaline assistant is 35%; stirring for 20-30min by a stirrer, completely and uniformly mixing, and then putting into a squeezer for squeezing, wherein the set pressure is 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 10-30 min, 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 1:3.5, 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 16%, 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, placing the boron nitride nanosheets in an alkaline solution, 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 nanosheets.

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

The embodiment also provides the white graphene cool composite fiber prepared by the method.

Example 5

A preparation method of a white graphene cool composite fiber comprises the following steps:

step 1, weighing the raw materials in proportion.

Preferably, each raw material comprises 85% of regenerated cellulose pulp, 14% of white graphene, 0.1% of modifier and 0.9% of alkaline assistant by mass percentage.

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

The modifier adopts a surfactant, comprises polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone and sodium dodecyl sulfate, and is prepared from the following raw materials in a mass ratio of 1: 2: 4: and 5, mixing.

Step 2, mixing the regenerated cellulose pulp with an aqueous solution of an alkaline assistant according to the mass ratio of 1:4, wherein the mass fraction of the aqueous solution of the alkaline assistant is 40%; stirring for 20-30min by a stirrer, completely and uniformly mixing, and then putting into a squeezer for squeezing, wherein the set pressure is 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 10-30 min, 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, placing the boron nitride nanosheets in an alkaline solution, 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 nanosheets.

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

The embodiment also provides the white graphene cool composite fiber prepared by the method.

The white graphene cool composite fibers prepared according to the embodiments of the present invention were tested, and the results are shown in table 1 below.

Table 1 test results.

The white graphene cool composite fiber and the preparation method thereof are characterized in that white graphene micro-sheets are added into regenerated cellulose fiber pulp, and a white graphene cool composite filament fiber is prepared by utilizing a white graphene micro-sheet preparation and dispersion system and improved regenerated cellulose spinning. Through the dispersion technology after optimizing, white graphite alkene realizes evenly distributed in the fibre, has excellent heat conduction function, can distribute away the heat that the human body produced rapidly, realizes human skin surface and cools down rapidly, makes human skin produce the cool sense of contact, and this composite fiber still has excellent antibacterial property simultaneously.

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.