阅读说明：本技术 一种功能性氨纶纤维的制备方法 (Preparation method of functional spandex fiber ) 是由 张满芬 曹雄飞 曹平 于 2021-08-12 设计创作，主要内容包括：本发明公开了一种功能性氨纶纤维的制备方法,该制备方法包括如下步骤：利用有机溶剂、A部分石墨烯或纳米碳纤维材料、聚醚二元醇,二异氰酸酯,得到预聚物溶液；预聚物溶液与和扩链溶液反应,熔体经过滤,再由纺丝设备纺丝,制备得到功能性氨纶纤维。本申请的氨纶纤维为多功能型,具有远红外、抑菌、高弹性、高强度、抗静电等特性,应用领域更广泛。(The invention discloses a preparation method of functional spandex fiber, which comprises the following steps: obtaining a prepolymer solution by using an organic solvent, a part A of graphene or carbon nanofiber material, polyether glycol and diisocyanate; and reacting the prepolymer solution with the chain extension solution, filtering the melt, and spinning by spinning equipment to prepare the functional spandex fiber. The spandex fiber is multifunctional, has the characteristics of far infrared, bacteriostasis, high elasticity, high strength, static resistance and the like, and is wider in application field.)

1. a preparation method of functional spandex fiber comprises the following steps:

1) preparation of prepolymer: adding an organic solvent, a part of graphene and/or carbon nanofiber material A and polyether glycol into diisocyanate according to the proportion of NCO/OH (NCO/OH) of 1.70-1.90; controlling the prepolymerization reaction temperature to be 70-80 ℃, controlling the reaction time to be 3.0-4 h, and introducing nitrogen for protection in the reaction process to obtain a prepolymer solution;

2) uniformly mixing part B of graphene and/or carbon nanofiber materials, zinc oxide nanoparticles and/or titanium dioxide nanoparticles, mixed amine and auxiliary material auxiliaries in an organic solvent to obtain a mixed amine solution;

3) the prepolymer solution and the chain extension solution are metered into a reaction kettle for mixing reaction, the temperature in the reaction kettle is heated to 150-208 ℃, the mixing reaction time is 45-48 minutes, the organic solvent is removed under reduced pressure after the reaction is finished, the raw materials reacted in the reaction kettle are directly conveyed to a melt filter for filtering, and the temperature in the melt filter is 218 +/-2 ℃;

5) continuously feeding the material filtered by the melt filter to a spinning box through two continuous metering conveying pumps, wherein the temperature in the spinning box is 215-218 ℃, and then spraying silk through a screen spinneret plate of a spinning box component; the aperture of the spinneret plate is 16 threads, and the density of the filter screen is 300 meshes;

6) cooling the sprayed strands through an air duct, wherein the air temperature is 25 ℃, and the air speed is 0.3 m/S; rheumatism is carried out at 51 ℃;

7) cooling an air channel, oiling by a 20HZ oil roller, then stretching guide wires by a guide wire roller, stretching the guide wires by the guide wire roller, then winding and forming in a winding machine at a winding speed of 580M/Min, dropping 4.6-5.5 denier high-elastic modulus spandex fiber yarns, then curing in a drying room at the curing temperature of 40 ℃ for 18 hours, and detecting after curing to prepare the functional spandex fiber;

the mass ratio of the part A graphene and/or nano carbon fiber material to the part B graphene and/or nano carbon fiber material is 3-5: 4-7.

2. The method for preparing functional spandex fiber according to claim 1, characterized in that: the polyether diol has a number average molecular weight of 2000-2500 and a molecular weight distribution of 1.4-1.5.

3. The method for preparing functional spandex fiber according to claim 1, characterized in that: the addition amount of the graphene or carbon nanofiber material accounts for 8-10% of the mass of the functional spandex fiber.

4. The method for preparing functional spandex fiber according to claim 1, characterized in that: the organic solvent is N, N-dimethylacetamide.

5. The method for preparing functional spandex fiber according to claim 1, characterized in that: the solid content of the prepolymer solution is 38-40%.

6. The method for preparing functional spandex fiber according to claim 1, characterized in that: the mixed amine is a mixture of two or more of ethylenediamine, propylenediamine, pentylenediamine and diethylamine.

7. The method for preparing functional spandex fiber according to claim 1, characterized in that: the other auxiliary material auxiliaries are as follows: one or more of an antioxidant, an anti-ultraviolet auxiliary agent, a dyeing auxiliary agent and a delustering agent.

8. The method for preparing functional spandex fiber according to claim 1, characterized in that: the godet roller is used for conducting godet wire stretching and is stretched by a four-stage godet roller, and the godet roller has the following parameters: lower godet roll 1: 14.86Hz, 140m/min, godet 1: 15.39Hz, 135 m/min; lower godet 2: 15.39Hz, 135m/min, godet 2: 15.39Hz, 135 m/min; lower godet roll 3: 15.92Hz, 150m/min, upper godet 3: 15.92Hz, 150 m/min; lower godet roll 4: 16.99Hz, 160m/min, upper godet roll 4: 16.99Hz and 160 m/min.

9. The method for preparing functional spandex fiber according to claim 1, characterized in that: the addition amount of the zinc oxide nano-particles and/or the titanium dioxide nano-particles accounts for 1-3% of the mass of the functional spandex fiber.

Technical Field

The invention relates to the technical field of chemical industry, in particular to a preparation method of functional spandex fiber.

Background

Spandex fibers have high elongation at break (above 400%), low modulus, and high elastic recovery, and are widely used. Besides higher strength, other physical and mechanical properties of the spandex fiber are very similar to those of natural latex yarn. But the strength of the composite material is 2-3 times higher than that of the latex yarn, the linear density is thinner, and the composite material is more resistant to chemical degradation. The spandex has better acid and alkali resistance, sweat resistance, seawater resistance, dry cleaning resistance and wear resistance, and can resist various dry cleaning agents and most of sun protection oil.

Currently, spandex fibers are generally used for most dyes and finishing agents of synthetic fibers and natural fibers, and are also suitable for dyeing and finishing spandex, but the application range of the spandex fibers has larger limitation. Based on the excellent performance, how to expand the application field and realize the maximization of the spandex fiber value becomes a problem to be solved urgently by the technical personnel in the field.

Disclosure of Invention

The technical problem to be solved by the invention is as follows: provides a preparation method of functional spandex fiber with various beneficial functions to human body.

In order to solve the technical problems, the technical scheme is as follows: a preparation method of functional spandex fiber comprises the following steps:

1) preparation of prepolymer: adding an organic solvent, a part of graphene and/or carbon nanofiber material A and polyether glycol into diisocyanate according to the proportion of NCO/OH (NCO/OH) of 1.70-1.90; controlling the prepolymerization reaction temperature to be 70-80 ℃, controlling the reaction time to be 3.0-4 h, and introducing nitrogen for protection in the reaction process to obtain a prepolymer solution;

2) uniformly mixing part B of graphene and/or carbon nanofiber materials, zinc oxide nanoparticles and/or titanium dioxide nanoparticles, mixed amine and auxiliary material auxiliaries in an organic solvent to obtain a mixed amine solution;

3) the prepolymer solution and the chain extension solution are metered into a reaction kettle for mixing reaction, the temperature in the reaction kettle is heated to 150-208 ℃, the mixing reaction time is 45-48 minutes, the organic solvent is removed under reduced pressure after the reaction is finished, the raw materials reacted in the reaction kettle are directly conveyed to a melt filter for filtering, and the temperature in the melt filter is 218 +/-2 ℃;

5) continuously feeding the material filtered by the melt filter to a spinning box through two continuous metering conveying pumps, wherein the temperature in the spinning box is 215-218 ℃, and then spraying silk through a screen spinneret plate of a spinning box component; the aperture of the spinneret plate is 16 threads, and the density of the filter screen is 300 meshes;

6) cooling the sprayed strands through an air duct, wherein the air temperature is 25 ℃, and the air speed is 0.3 m/S; rheumatism is carried out at 51 ℃;

7) cooling an air channel, oiling by a 20HZ oil roller, then stretching guide wires by a guide wire roller, stretching the guide wires by the guide wire roller, then winding and forming in a winding machine at a winding speed of 580M/Min, dropping 4.6-5.5 denier high-elastic modulus spandex fiber yarns, then curing in a drying room at the curing temperature of 40 ℃ for 18 hours, and detecting after curing to prepare the functional spandex fiber;

the mass ratio of the part A graphene and/or nano carbon fiber material to the part B graphene and/or nano carbon fiber material is 3-5: 4-7.

The polyether diol has a number average molecular weight of 2000-2500 and a molecular weight distribution of 1.4-1.5.

The addition amount of the graphene or carbon nanofiber material accounts for 8-10% of the mass of the functional spandex fiber.

The organic solvent is N, N-dimethylacetamide.

The solid content of the prepolymer solution is 38-40%.

The mixed amine is a mixture of two or more of ethylenediamine, propylenediamine, pentylenediamine and diethylamine.

The other auxiliary material auxiliaries are as follows: one or more of an antioxidant, an anti-ultraviolet auxiliary agent, a dyeing auxiliary agent and a delustering agent.

The godet roller is used for conducting godet wire stretching and is stretched by a four-stage godet roller, and the godet roller has the following parameters: lower godet roll 1: 14.86Hz, 140m/min, godet 1: 15.39Hz, 135 m/min; lower godet 2: 15.39Hz, 135m/min, godet 2: 15.39Hz, 135 m/min; lower godet roll 3: 15.92Hz, 150m/min, upper godet 3: 15.92Hz, 150 m/min; lower godet roll 4: 16.99Hz, 160m/min, upper godet roll 4: 16.99Hz and 160 m/min.

The addition amount of the zinc oxide nano-particles and/or the titanium dioxide nano-particles accounts for 1-3% of the mass of the functional spandex fiber.

Has the advantages that: according to the invention, a mode of adding the graphene material step by step is adopted, so that the graphene material is respectively embedded in a plurality of dimensions such as an oligomer molecule, a polymer molecule and a polymer surface, the graphene is promoted to form buffer connection points of the graphene on a fiber molecular chain, between chains and on the fiber surface, so that the graphene is connected in series from micro to macro by the graphene in the fiber molecule and between molecules, the excellent performances of the graphene and the graphene are fully exerted, and the fiber formed by compounding the graphene and the graphene has more excellent mechanical performances, especially breaking strength, compared with the traditional spandex fiber.

After the nano particles are fixed on spandex fibers, the obtained modified spandex fibers obtain good antibacterial performance of the nano particles such as zinc oxide and titanium dioxide, and the modified spandex fiber material with good hydrophilicity and antibacterial performance is obtained by combining the excellent performance of the spandex fibers.

The spandex fiber is multifunctional, has the characteristics of far infrared, bacteriostasis, high elasticity, high strength, static resistance and the like, and is wider in application field.

Detailed Description

The process of the present invention is further illustrated below, but is not limited thereto.

Example 1

The preparation method of the functional spandex fiber comprises the following steps:

1) preparation of prepolymer: adding diisocyanate into N, N-dimethylacetamide, partial graphene A and polyether glycol according to the proportion of NCO/OH (NCO/OH) of 1.70-1.90; controlling the prepolymerization reaction temperature to be 70-80 ℃, controlling the reaction time to be 3.0-4 h, and introducing nitrogen for protection in the reaction process to obtain a prepolymer solution with the solid content of 38-40%; the polyether diol has a number average molecular weight of 2000-2500 and a molecular weight distribution of 1.4-1.5.

2) Uniformly mixing part B of graphene, zinc oxide nanoparticles and/or titanium dioxide nanoparticles, mixed amine and auxiliary material auxiliaries in N, N-dimethylacetamide to obtain a mixed amine solution;

the addition amount of the zinc oxide nano-particles and/or the titanium dioxide nano-particles accounts for 2% of the mass of the functional spandex fiber;

the addition amount of the graphene accounts for 10% of the mass of the functional spandex fiber;

the mass ratio of the part A graphene to the part B graphene is 5: 7;

3) the prepolymer solution and the chain extension solution are metered into a reaction kettle for mixing reaction, the temperature in the reaction kettle is heated to 150-208 ℃, the mixing reaction time is 45-48 minutes, the reaction is finished, N-dimethylacetamide is removed through decompression, the raw materials reacted in the reaction kettle are directly conveyed to a melt filter for filtering, and the temperature in the melt filter is 218 +/-2 ℃;

5) continuously feeding the material filtered by the melt filter to a spinning box through two continuous metering conveying pumps, wherein the temperature in the spinning box is 215-218 ℃, and then spraying silk through a screen spinneret plate of a spinning box component; the aperture of the spinneret plate is 16 threads, and the density of the filter screen is 300 meshes;

6) cooling the sprayed strands through an air duct, wherein the air temperature is 25 ℃, and the air speed is 0.3 m/S; rheumatism is carried out at 51 ℃;

7) after cooling, the air channel is oiled by a 20HZ oil roller, then the godet roller is used for conducting godet wire stretching, and the lower godet roller is 1: 14.86Hz, 140m/min, godet 1: 15.39Hz, 135 m/min; lower godet 2: 15.39Hz, 135m/min, godet 2: 15.39Hz, 135 m/min; lower godet roll 3: 15.92Hz, 150m/min, upper godet 3: 15.92Hz, 150 m/min; lower godet roll 4: 16.99Hz, 160m/min, upper godet roll 4: 16.99Hz, 160 m/min; after being stretched by a yarn guide roller, the spandex filaments enter a winding machine for winding and forming, the winding speed of the winding machine is 580M/Min, 4.6-5.5 denier of high-elastic modulus spandex filaments fall into a drying room for curing, the curing temperature is 40 ℃, the curing time is 18 hours, and after curing, detection is carried out to prepare functional spandex fibers;

the mixed amine is a mixture of ethylenediamine and propylenediamine.

The other auxiliary material auxiliary agents are as follows: antioxidant, uvioresistant assistant and dyeing assistant.

Example 2

The preparation method of the functional spandex fiber comprises the following steps:

1) preparation of prepolymer: adding N, N-dimethylacetamide, part A of the carbon nanofiber material and polyether glycol into diisocyanate according to the proportion of NCO/OH (NCO/OH) of 1.70-1.90; controlling the prepolymerization reaction temperature to be 70-80 ℃, controlling the reaction time to be 3.0-4 h, and introducing nitrogen for protection in the reaction process to obtain a prepolymer solution with the solid content of 38-40%; the polyether diol has a number average molecular weight of 2000-2500 and a molecular weight distribution of 1.4-1.5

2) Uniformly mixing the part B of the carbon nanofiber material, the zinc oxide nanoparticles and/or the titanium dioxide nanoparticles, the mixed amine and the auxiliary material auxiliary agent in N, N-dimethylacetamide to obtain a mixed amine solution;

the mass ratio of the part A of nano carbon fiber materials to the part B of nano carbon fiber materials is 3: 7;

the addition amount of the nano carbon fiber material accounts for 9 percent of the mass of the functional spandex fiber; the addition amount of the zinc oxide nano-particles and/or the titanium dioxide nano-particles accounts for 3% of the mass of the functional spandex fiber;

3) the prepolymer solution and the chain extension solution are metered into a reaction kettle for mixing reaction, the temperature in the reaction kettle is heated to 150-208 ℃, the mixing reaction time is 45-48 minutes, the reaction is finished, N-dimethylacetamide is removed through decompression, the raw materials reacted in the reaction kettle are directly conveyed to a melt filter for filtering, and the temperature in the melt filter is 218 +/-2 ℃;

5) continuously feeding the material filtered by the melt filter to a spinning box through two continuous metering conveying pumps, wherein the temperature in the spinning box is 215-218 ℃, and then spraying silk through a screen spinneret plate of a spinning box component; the aperture of the spinneret plate is 16 threads, and the density of the filter screen is 300 meshes;

6) cooling the sprayed strands through an air duct, wherein the air temperature is 25 ℃, and the air speed is 0.3 m/S; rheumatism is carried out at 51 ℃;

7) after cooling, the air channel is oiled by a 20HZ oil roller, then the godet roller is used for conducting godet wire stretching, and the lower godet roller is 1: 14.86Hz, 140m/min, godet 1: 15.39Hz, 135 m/min; lower godet 2: 15.39Hz, 135m/min, godet 2: 15.39Hz, 135 m/min; lower godet roll 3: 15.92Hz, 150m/min, upper godet 3: 15.92Hz, 150 m/min; lower godet roll 4: 16.99Hz, 160m/min, upper godet roll 4: 16.99Hz, 160 m/min; after being stretched by a yarn guide roller, the spandex filaments enter a winding machine for winding and forming, the winding speed of the winding machine is 580M/Min, 4.6-5.5 denier of high-elastic modulus spandex filaments fall into a drying room for curing, the curing temperature is 40 ℃, the curing time is 18 hours, and after curing, detection is carried out to prepare functional spandex fibers;

the mixed amine is a mixture of ethylenediamine and pentanediamine.

The other auxiliary material auxiliary agents are as follows: antioxidant, anti-ultraviolet assistant, dyeing assistant and flatting agent.

Example 3

The only difference from example 1 is: in the step 1) and the step 2), a mixture of graphene and carbon nanofiber materials in any proportion is added, and the addition amount of the graphene and the carbon nanofiber materials accounts for 8% of the mass of the functional spandex fiber.

Example 4

The difference from example 1 is only that the addition amount of zinc oxide nanoparticles and/or titanium dioxide nanoparticles is adjusted to 1% of the mass of the functional spandex fiber.

The functional fibers obtained in examples 1 to 4 were subjected to a performance test, and the test results are shown in the following table: