阅读说明：本技术 一种白石墨烯复合再生涤纶短纤及其制备方法 (White graphene composite regenerated polyester staple fiber and preparation method thereof ) 是由 马立国 沙嫣 沙晓林 于 2021-07-22 设计创作，主要内容包括：本发明公开了一种白石墨烯复合再生涤纶短纤及其制备方法,该方法包含：步骤1,按比例称取各原料；步骤2,将再生涤纶切片及白石墨烯分别进行干燥处理,然后将再生涤纶切片和白石墨烯以及改性剂混合搅拌,得到白石墨烯再生涤纶混合物；步骤3,将步骤2所得的白石墨烯再生涤纶混合物加入到双螺杆挤出机中挤出造粒,得到改性白石墨烯再生涤纶母粒；步骤4,将步骤3所得的改性白石墨烯再生涤纶母粒进行干燥,然后加入到螺杆挤出机中加热熔融,再经纺丝箱体过滤后纺丝成束。本发明还提供了该方法制备的白石墨烯复合再生涤纶短纤。本发明制备的纤维具有抗菌、远红外、抗紫外特点,且该纤维中白石墨烯分散均匀,不易脱落,功能性具有持久性。(The invention discloses a white graphene composite regenerated polyester staple fiber and a preparation method thereof, wherein the method comprises the following steps: step 1, weighing raw materials in proportion; step 2, respectively drying the regenerated polyester chips and the white graphene, and then mixing and stirring the regenerated polyester chips, the white graphene and the modifier to obtain a white graphene regenerated polyester mixture; step 3, adding the white graphene regenerated polyester mixture obtained in the step 2 into a double-screw extruder for extrusion granulation to obtain modified white graphene regenerated polyester master batches; and 4, drying the modified white graphene regenerated polyester master batch obtained in the step 3, adding the dried modified white graphene regenerated polyester master batch into a screw extruder for heating and melting, filtering the mixture by a spinning manifold, and spinning the mixture into bundles. The invention also provides the white graphene composite regenerated polyester staple fiber prepared by the method. The fiber prepared by the method has the characteristics of antibiosis, far infrared and ultraviolet resistance, and the white graphene in the fiber is uniformly dispersed and is not easy to fall off, so that the functionality is durable.)

1. The preparation method of the white graphene composite regenerated polyester staple fiber is characterized by comprising the following steps:

step 1, weighing raw materials in proportion; the raw materials comprise regenerated polyester chips, white graphene and a modifier;

step 2, respectively drying the regenerated polyester chips and the white graphene, and then mixing and stirring the regenerated polyester chips, the white graphene and the modifier to obtain a white graphene regenerated polyester mixture;

step 3, adding the white graphene regenerated polyester mixture obtained in the step 2 into a double-screw extruder for extrusion granulation to obtain modified white graphene regenerated polyester master batches;

and 4, drying the modified white graphene regenerated polyester master batch obtained in the step 3, adding the dried modified white graphene regenerated polyester master batch into a screw extruder for heating and melting, filtering the obtained product by a spinning box, and then spinning the product into bundles to obtain the white graphene composite regenerated polyester staple fibers.

2. The preparation method of the white graphene composite regenerated polyester staple fiber according to claim 1, wherein the raw materials comprise, by mass: 84-99% of regenerated polyester chips, 0.1-15% of white graphene and 0.1-1% of modifier.

3. The preparation method of the white graphene composite regenerated polyester staple fiber as claimed in claim 2, wherein the modifier is polyvinyl alcohol, hydroxypropyl cellulose, sodium lignosulfonate, silane coupling agent in a mass ratio of 1: (1-2): (2-4): (3-5).

4. The method for preparing the white graphene composite regenerated polyester staple fibers according to claim 2, wherein the white graphene is prepared by any one of a borax-ammonium chloride method, a chemical vapor deposition method, a borax-urea method, a high-frequency plasma method, a hydrothermal method and a precursor method.

5. The method for preparing the white graphene composite regenerated polyester staple fiber as claimed in claim 1, wherein in the step 2, the regenerated polyester chip and the white graphene are respectively dried, and the water content of both the dried regenerated polyester chip and the dried white graphene is less than 100 ppm.

6. The preparation method of the white graphene composite regenerated polyester staple fiber as claimed in claim 1, wherein in the step 2, the regenerated polyester chips, the white graphene and the modifier are placed into a high-speed mixer for mixing and stirring, the mixing and stirring speed is 1000-3000 r/min, and the stirring time is 30-50 min.

7. The method for preparing the white graphene composite regenerated polyester staple fiber as claimed in claim 1, wherein in the step 3, the temperature ranges from the first zone to the fifth zone of the twin-screw extruder are respectively 250-.

8. The method for preparing the white graphene composite regenerated polyester staple fiber according to claim 1, wherein in the step 4, the modified white graphene regenerated polyester master batch is dried at a drying temperature of 50-150 ℃, and the water content of the dried master batch is less than 100 ppm.

9. The method for preparing the white graphene composite regenerated polyester staple fiber as claimed in claim 1, wherein in the step 4, the spinning temperature is 290-310 ℃, and the spinning speed is 1500-2000 m/min.

10. The white graphene composite regenerated polyester staple fiber prepared by the method of any one of 1-9.

Technical Field

The invention relates to a white graphene regenerated polyester composite fiber and a preparation method thereof, and particularly relates to a white graphene regenerated polyester staple 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, far infrared, ultraviolet-resistant and other performances, and has great development potential in fiber application.

At present, the annual output of textile fibers such as terylene is large, a large amount of waste terylene fabrics are eliminated every year, not only serious pollution is caused, but also a large amount of petroleum resources are wasted, and the petroleum and other data can not be regenerated, so that the terylene fibers are necessary to be recycled.

Disclosure of Invention

The invention aims to provide a white graphene regenerated polyester composite fiber and a preparation method thereof, and the prepared fusion method modified white graphene regenerated polyester composite fiber has the functions of antibiosis, mite prevention, ultraviolet resistance, far infrared resistance and the like, improves the additional value of polyester, and expands the application range of the regenerated polyester fiber.

In order to achieve the above object, the present invention provides a method for preparing a white graphene composite regenerated polyester staple fiber, wherein the method comprises: step 1, weighing raw materials in proportion; the raw materials comprise regenerated polyester chips, white graphene and a modifier; step 2, respectively drying the regenerated polyester chips and the white graphene, and then mixing and stirring the regenerated polyester chips, the white graphene and the modifier to obtain a white graphene regenerated polyester mixture; step 3, adding the white graphene regenerated polyester mixture obtained in the step 2 into a double-screw extruder for extrusion granulation to obtain modified white graphene regenerated polyester master batches; and 4, drying the modified white graphene regenerated polyester master batch obtained in the step 3, adding the dried modified white graphene regenerated polyester master batch into a screw extruder for heating and melting, filtering the obtained product by a spinning box, and then spinning the product into bundles to obtain the white graphene composite regenerated polyester staple fibers.

The preparation method of the white graphene composite regenerated polyester staple fiber comprises the following raw materials in percentage by mass: 84-99% of regenerated polyester chips, 0.1-15% of white graphene and 0.1-1% of modifier.

The preparation method of the white graphene composite regenerated polyester staple fiber comprises the following steps of (1): (1-2): (2-4): (3-5).

The preparation method of the white graphene composite regenerated polyester staple fiber comprises the step of preparing the white graphene by any one of a borax-ammonium chloride method, a chemical vapor deposition method, a borax-urea method, a high-frequency plasma method, a hydrothermal method and a precursor method.

In the step 2, the regenerated polyester chips and the white graphene are respectively dried, and the water content of both the dried regenerated polyester chips and the dried white graphene is less than 100 ppm.

In the step 2, the regenerated polyester chips, the white graphene and the modifier are mixed and stirred in a high-speed mixer, wherein the mixing and stirring speed is 1000-3000 r/min, and the stirring time is 30-50 min.

In the step 3, the temperature ranges from the first zone to the fifth zone of the twin-screw extruder are respectively 250-.

In the step 4, the modified white graphene regenerated polyester master batch is dried at the drying temperature of 50-150 ℃, and the water content of the dried master batch is less than 100 ppm.

In the preparation method of the white graphene composite regenerated polyester staple fiber, in the step 4, the spinning temperature is 290-fold and 310 ℃, and the spinning speed is 1500-fold and 2000 m/min.

The invention also provides the white graphene composite regenerated polyester staple fiber prepared by the method.

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

the white graphene regenerated polyester fiber prepared by the melting method has excellent performances of antibiosis, mite prevention, far infrared, ultraviolet resistance and the like, wherein the bacteriostasis rate of escherichia coli, staphylococcus aureus and candida albicans reaches 99.9%, the mite inhibition rate is more than 90%, the far infrared temperature rise reaches 0.88, the UPF is more than 100, and the functionality is good.

The method preferentially prepares the white graphene regenerated polyester master batch, and then prepares the modified white graphene regenerated polyester composite fiber by carrying out melt spinning on the white graphene regenerated polyester master batch, so that the method is simple in process, easy to operate, low in cost, high in economic benefit and 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 composite regenerated polyester staple fibers, which comprises the following steps: step 1, weighing raw materials in proportion; the raw materials comprise regenerated polyester chips, white graphene and a modifier; step 2, respectively drying the regenerated polyester chips and the white graphene, and then mixing and stirring the regenerated polyester chips, the white graphene and the modifier to obtain a white graphene regenerated polyester mixture; step 3, adding the white graphene regenerated polyester mixture obtained in the step 2 into a double-screw extruder for extrusion granulation to obtain modified white graphene regenerated polyester master batches; and 4, drying the modified white graphene regenerated polyester master batch obtained in the step 3, adding the dried modified white graphene regenerated polyester master batch into a screw extruder for heating and melting, filtering the obtained product by a spinning box, and then spinning the product into bundles to obtain the white graphene composite regenerated polyester staple fibers.

The regenerated polyester staple fibers are prepared by using polyester cloth, waste polyester bottle chips, waste spinning yarns, bubble materials and pulp blocks as raw materials, crushing and cleaning the waste polyester bottle chips, processing a mixture of various materials into regenerated polyester chips, drying, melt extruding, spinning, winding, bundling, drafting, curling (meanwhile, adding different oil agents according to requirements during curling), relaxing, heat setting and cutting.

Preferably, each raw material comprises the following components in percentage by mass: 84-99% of regenerated polyester chips, 0.1-15% of white graphene and 0.1-1% of modifier.

The modifier is polyvinyl alcohol, hydroxypropyl cellulose, sodium lignin sulfonate and a silane coupling agent in a mass ratio of 1: (1-2): (2-4): (3-5).

The white graphene is prepared by any one of a borax-ammonium chloride method, a chemical vapor deposition method, a borax-urea method, a high-frequency plasma method, a hydrothermal method, a precursor method and the like.

And 2, respectively drying the regenerated polyester chips and the white graphene, wherein the water content of the dried regenerated polyester chips and the water content of the dried white graphene are both less than 100 ppm.

And 2, putting the regenerated polyester chips, the white graphene and the modifier into a high-speed mixer for mixing and stirring, wherein the mixing and stirring speed is 1000-3000 r/min, and the stirring time is 30-50 min.

In the step 2, the dried regenerated polyester chips can be ground to obtain regenerated polyester chip powder, the particle size of the powder is less than 100 microns, and then the white graphene powder and the modifier are added into the regenerated polyester chip powder to be mixed and stirred to obtain the white graphene regenerated polyester mixed powder.

In step 3, the temperature ranges from the first zone to the fifth zone of the double-screw extruder are respectively 250-.

And 4, drying the modified white graphene regenerated polyester master batch at the drying temperature of 50-150 ℃, wherein the water content of the dried master batch is less than 100 ppm.

In the step 4, the spinning temperature is 290-310 ℃, and the spinning speed is 1500-2000 m/min.

The equipment used in the present invention is known to those skilled in the art.

The invention also provides the white graphene composite regenerated polyester staple fiber prepared by the method.

The white graphene composite regenerated polyester staple fiber and the preparation method thereof provided by the invention are further described below with reference to the examples.

Example 1

A preparation method of white graphene composite regenerated polyester staple fibers comprises the following steps:

step 1, weighing raw materials in proportion; the raw materials comprise regenerated polyester chips, white graphene and a modifier.

Preferably, each raw material comprises the following components in percentage by mass: 99% of regenerated polyester chips, 0.1% of white graphene and 0.9% of modifier.

The modifier is polyvinyl alcohol, hydroxypropyl cellulose, sodium lignin sulfonate and a silane coupling agent in a mass ratio of 1: 1: 2: 3, and (b) a mixture of the components.

The white graphene is prepared by adopting a borax-ammonium chloride method.

Step 2, respectively drying the regenerated polyester chips and the white graphene, wherein the water content of the dried regenerated polyester chips and the water content of the dried white graphene are both less than 100 ppm; and then placing the regenerated polyester chips, the white graphene and the modifier into a high-speed mixer for mixing and stirring, wherein the mixing and stirring speed is 1000-3000 r/min, and the stirring time is 30-50 min, so as to obtain a white graphene regenerated polyester mixture.

And 3, adding the white graphene regenerated polyester mixture obtained in the step 2 into a double-screw extruder for extrusion granulation to obtain the modified white graphene regenerated polyester master batch. The temperature ranges from the first zone to the fifth zone of the double-screw extruder are respectively 250-260 ℃, 255-265 ℃, 260-270 ℃, 255-265 ℃ and 250-260 ℃.

Step 4, drying the modified white graphene regenerated polyester master batch obtained in the step 3, wherein the drying temperature is 50-150 ℃, and the water content of the dried master batch is less than 100 ppm; and then adding the mixture into a screw extruder for heating and melting, filtering the mixture through a spinning box, and spinning the mixture into bundles at the spinning temperature of 290-plus-310 ℃ and the spinning speed of 1500-plus-2000 m/min to obtain the white graphene composite regenerated polyester staple fiber.

The embodiment also provides the white graphene composite regenerated polyester staple fiber prepared by the method.

Example 2

A preparation method of white graphene composite regenerated polyester staple fibers comprises the following steps:

step 1, weighing raw materials in proportion; the raw materials comprise regenerated polyester chips, white graphene and a modifier.

Preferably, each raw material comprises the following components in percentage by mass: 94.7% of regenerated polyester chips, 5% of white graphene and 0.3% of modifier.

The modifier is polyvinyl alcohol, hydroxypropyl cellulose, sodium lignin sulfonate and a silane coupling agent in a mass ratio of 1: 1: 2.5: 3.5.

The white graphene is prepared by adopting a chemical vapor deposition method.

Step 2, respectively drying the regenerated polyester chips and the white graphene, wherein the water content of the dried regenerated polyester chips and the water content of the dried white graphene are both less than 100 ppm; and then placing the regenerated polyester chips, the white graphene and the modifier into a high-speed mixer for mixing and stirring, wherein the mixing and stirring speed is 1000-3000 r/min, and the stirring time is 30-50 min, so as to obtain a white graphene regenerated polyester mixture.

And 3, adding the white graphene regenerated polyester mixture obtained in the step 2 into a double-screw extruder for extrusion granulation to obtain the modified white graphene regenerated polyester master batch. The temperature ranges from the first zone to the fifth zone of the double-screw extruder are respectively 250-260 ℃, 255-265 ℃, 260-270 ℃, 255-265 ℃ and 250-260 ℃.

Step 4, drying the modified white graphene regenerated polyester master batch obtained in the step 3, wherein the drying temperature is 50-150 ℃, and the water content of the dried master batch is less than 100 ppm; and then adding the mixture into a screw extruder for heating and melting, filtering the mixture through a spinning box, and spinning the mixture into bundles at the spinning temperature of 290-plus-310 ℃ and the spinning speed of 1500-plus-2000 m/min to obtain the white graphene composite regenerated polyester staple fiber.

The embodiment also provides the white graphene composite regenerated polyester staple fiber prepared by the method.

Example 3

A preparation method of white graphene composite regenerated polyester staple fibers comprises the following steps:

step 1, weighing raw materials in proportion; the raw materials comprise regenerated polyester chips, white graphene and a modifier.

Preferably, each raw material comprises the following components in percentage by mass: 91.9% of regenerated polyester chips, 8% of white graphene and 0.1% of modifier.

The modifier is polyvinyl alcohol, hydroxypropyl cellulose, sodium lignin sulfonate and a silane coupling agent in a mass ratio of 1: 1.5: 3: 4, and (b) a mixture of the components.

The white graphene is prepared by adopting a borax-urea method.

Step 2, respectively drying the regenerated polyester chips and the white graphene, wherein the water content of the dried regenerated polyester chips and the water content of the dried white graphene are both less than 100 ppm; and then placing the regenerated polyester chips, the white graphene and the modifier into a high-speed mixer for mixing and stirring, wherein the mixing and stirring speed is 1000-3000 r/min, and the stirring time is 30-50 min, so as to obtain a white graphene regenerated polyester mixture.

And 3, adding the white graphene regenerated polyester mixture obtained in the step 2 into a double-screw extruder for extrusion granulation to obtain the modified white graphene regenerated polyester master batch. The temperature ranges from the first zone to the fifth zone of the double-screw extruder are respectively 250-260 ℃, 255-265 ℃, 260-270 ℃, 255-265 ℃ and 250-260 ℃.

Step 4, drying the modified white graphene regenerated polyester master batch obtained in the step 3, wherein the drying temperature is 50-150 ℃, and the water content of the dried master batch is less than 100 ppm; and then adding the mixture into a screw extruder for heating and melting, filtering the mixture through a spinning box, and spinning the mixture into bundles at the spinning temperature of 290-plus-310 ℃ and the spinning speed of 1500-plus-2000 m/min to obtain the white graphene composite regenerated polyester staple fiber.

The embodiment also provides the white graphene composite regenerated polyester staple fiber prepared by the method.

Example 4

A preparation method of white graphene composite regenerated polyester staple fibers comprises the following steps:

step 1, weighing raw materials in proportion; the raw materials comprise regenerated polyester chips, white graphene and a modifier.

Preferably, each raw material comprises the following components in percentage by mass: 87.5% of regenerated polyester chips, 12% of white graphene and 0.5% of modifier.

The modifier is polyvinyl alcohol, hydroxypropyl cellulose, sodium lignin sulfonate and a silane coupling agent in a mass ratio of 1: 2: 3.5: 4.5 of the composition.

The white graphene is prepared by adopting a high-frequency plasma method.

Step 2, respectively drying the regenerated polyester chips and the white graphene, wherein the water content of the dried regenerated polyester chips and the water content of the dried white graphene are both less than 100 ppm; and then placing the regenerated polyester chips, the white graphene and the modifier into a high-speed mixer for mixing and stirring, wherein the mixing and stirring speed is 1000-3000 r/min, and the stirring time is 30-50 min, so as to obtain a white graphene regenerated polyester mixture.

And 3, adding the white graphene regenerated polyester mixture obtained in the step 2 into a double-screw extruder for extrusion granulation to obtain the modified white graphene regenerated polyester master batch. The temperature ranges from the first zone to the fifth zone of the double-screw extruder are respectively 250-260 ℃, 255-265 ℃, 260-270 ℃, 255-265 ℃ and 250-260 ℃.

Step 4, drying the modified white graphene regenerated polyester master batch obtained in the step 3, wherein the drying temperature is 50-150 ℃, and the water content of the dried master batch is less than 100 ppm; and then adding the mixture into a screw extruder for heating and melting, filtering the mixture through a spinning box, and spinning the mixture into bundles at the spinning temperature of 290-plus-310 ℃ and the spinning speed of 1500-plus-2000 m/min to obtain the white graphene composite regenerated polyester staple fiber.

The embodiment also provides the white graphene composite regenerated polyester staple fiber prepared by the method.

Example 5

A preparation method of white graphene composite regenerated polyester staple fibers comprises the following steps:

step 1, weighing raw materials in proportion; the raw materials comprise regenerated polyester chips, white graphene and a modifier.

Preferably, each raw material comprises the following components in percentage by mass: 84% of regenerated polyester chips, 15% of white graphene and 1% of modifier.

The modifier is polyvinyl alcohol, hydroxypropyl cellulose, sodium lignin sulfonate and a silane coupling agent in a mass ratio of 1: 2: 4: 5, and (c) a mixture of the components.

The white graphene is prepared by a hydrothermal method or a precursor method.

Step 2, respectively drying the regenerated polyester chips and the white graphene, wherein the water content of the dried regenerated polyester chips and the water content of the dried white graphene are both less than 100 ppm; and then placing the regenerated polyester chips, the white graphene and the modifier into a high-speed mixer for mixing and stirring, wherein the mixing and stirring speed is 1000-3000 r/min, and the stirring time is 30-50 min, so as to obtain a white graphene regenerated polyester mixture.

And 3, adding the white graphene regenerated polyester mixture obtained in the step 2 into a double-screw extruder for extrusion granulation to obtain the modified white graphene regenerated polyester master batch. The temperature ranges from the first zone to the fifth zone of the double-screw extruder are respectively 250-260 ℃, 255-265 ℃, 260-270 ℃, 255-265 ℃ and 250-260 ℃.

Step 4, drying the modified white graphene regenerated polyester master batch obtained in the step 3, wherein the drying temperature is 50-150 ℃, and the water content of the dried master batch is less than 100 ppm; and then adding the mixture into a screw extruder for heating and melting, filtering the mixture through a spinning box, and spinning the mixture into bundles at the spinning temperature of 290-plus-310 ℃ and the spinning speed of 1500-plus-2000 m/min to obtain the white graphene composite regenerated polyester staple fiber.

The embodiment also provides the white graphene composite regenerated polyester staple fiber prepared by the method.

The finished products from the examples were tested for functionality and the results are shown in table 1 below.

TABLE 1 test results.

The invention provides a white graphene composite regenerated polyester staple fiber and a preparation method thereof, and aims to prepare a modified white graphene regenerated polyester staple fiber by using a modified white graphene dispersion system and a regenerated polyester melting method technology. The characteristic technology is that a modified white graphene regenerated polyester master batch is preferentially prepared, and then melt spinning is carried out on the dried master batch to prepare the white graphene regenerated polyester staple fiber. The fiber has the characteristics of antibiosis, far infrared and ultraviolet resistance, and the white graphene in the white graphene regenerated polyester staple fiber is uniformly dispersed and not easy to fall off, and the functionality has durability.

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.