CN112127000B - Far infrared acrylic fiber and preparation method thereof - Google Patents
Far infrared acrylic fiber and preparation method thereof Download PDFInfo
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- CN112127000B CN112127000B CN202010919616.4A CN202010919616A CN112127000B CN 112127000 B CN112127000 B CN 112127000B CN 202010919616 A CN202010919616 A CN 202010919616A CN 112127000 B CN112127000 B CN 112127000B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/54—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of unsaturated nitriles
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/42—Nitriles
- C08F220/44—Acrylonitrile
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
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Abstract
The invention discloses a far infrared acrylic fiber and a preparation method thereof, wherein the emissivity of the far infrared acrylic fiber at the wavelength of 4-14 mu m is 0.82-0.87. The far infrared acrylic fiber is prepared by the following method: (1) Mixing the far infrared component and polyethylene glycol, and grinding and dispersing into far infrared slurry under ultrasonic conditions; (2) Adding a reaction monomer into far infrared slurry, simultaneously adding a catalyst, an accelerator, an activator, an acid agent and a dispersing agent, and carrying out in-situ polymerization reaction on the monomer among the far infrared nanometer molecular structure layers to obtain far infrared polymer slurry, and carrying out single removal, filtration and drying on the slurry to obtain a far infrared polymer; (3) Dissolving far infrared polymer in dimethylacetamide to obtain glue solution, and carrying out wet solution spinning to obtain the far infrared acrylic fiber. The invention adopts an in-situ polymerization mode to prepare the far infrared acrylic fiber by a wet two-step acrylic process method, so as to ensure that the product has long far infrared emission performance and better mechanical stability.
Description
Technical Field
The invention belongs to the technical field of functional fibers, and particularly relates to a far infrared acrylic fiber and a preparation method thereof.
Background
Along with the improvement of life quality of people, demands for functional fiber products are rapidly increased, and the far infrared acrylic fiber is a novel functional fiber with the function of absorbing and emitting far infrared electromagnetic waves. The acrylic fiber compounded with nano inorganic far infrared health-care components can emit high far infrared electromagnetic waves with the wavelength corresponding to the absorption of human body radiation, is a good far infrared radiation material for human body health care, has the functions of resisting ultraviolet rays, sterilizing, eliminating peculiar smell and the like, can effectively improve human body microcirculation, improve tissue oxygen supply, activate tissue cells, improve metabolism, prevent aging, strengthen an immune system and the like. The far infrared acrylic fiber also has excellent moth resistance, good fluffiness and comfort, has a hand feel similar to wool, and the comfort and the air permeability of the wear are more in line with the demands of people. Therefore, the method has strong development advantages in the application fields of textile products such as gloves, cushions, sweaters, scarves, quilts and the like.
The main mode of the preparation of the far infrared functional acrylic fiber at present is a solution blending spinning method in the process of preparing glue from stock solution and spinning, namely, the far infrared fiber is prepared by a ceramic particle with the far infrared radiation function and a conventional polymer blending melt spinning method; the method can also be used for coating post-treatment of forming fabrics, and the far infrared function is realized by mixing and coating far infrared nano powder into the fiber, so that the produced far infrared acrylic fiber only macroscopically increases far infrared components, and the uniformity and stability of the far infrared function of the fiber have defects, and the far infrared acrylic textile product prepared by the method can also cause the far infrared function to be weakened to a certain extent in the use process, thereby reducing the far infrared emissivity and reducing the far infrared efficacy.
The mode of making far infrared acrylic fiber more advanced and stable and durable than the solution blending yarn method is that the molecular structure of the polyacrylonitrile polymer used for producing acrylic fiber is changed by an in-situ polymerization method, thereby realizing the purpose that the far infrared acrylic fiber produced by the wet process has the function of continuous electromagnetic wave emission.
The research and development of far infrared technology at normal temperature in Japan is at the international leading level, and according to the description of Japanese patent, the emissivity of ceramic powder selected for far infrared textiles at normal temperature is generally more than 0.65, preferably more than 0.75, and most preferably more than 0.90. In-situ polymerization can realize the modification of the molecular structure of the polymer by adding nano material components. Because of complex in-situ polymerization reaction, the particle size of the added ceramic powder with far infrared function and the selection technical requirement of the dispersing agent are high, otherwise, the spinning difficulty can be caused to influence the quality of fibers, and the aggregation can be caused to influence the progress of the polymerization reaction after the dispersion. The current technical data and reports of in-situ polymerization reaction for acrylic fiber are less, and are limited to laboratory researches, and no comparative system, mature research data and market production examples exist.
In view of this, the present invention has been made.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a far infrared acrylic fiber and a preparation method thereof, wherein the preparation method is characterized in that far infrared components are dispersed in advance to form far infrared slurry with a plurality of gaps among molecules, so that a redox system is formed in the far infrared slurry by subsequently added reaction monomers and reaction reagents, and subsequent in-situ polymerization reaction is completed, so that the product has long far infrared emission performance and better mechanical stability.
In order to solve the technical problems, the invention adopts the basic conception of the technical scheme that:
the invention provides far infrared acrylic fiber, wherein the emissivity of the far infrared acrylic fiber at the wavelength of 4-14 mu m is 0.82-0.89.
In the scheme, the far infrared acrylic fiber has higher emissivity in the range of the optimal infrared absorption wavelength of a human body. As the far infrared component is introduced into the acrylic fiber in an in-situ polymerization mode, compared with the scheme that the far infrared component is directly added into the acrylic spinning solution in the prior art or is coated on the surface of the fiber, the acrylic fiber provided by the application has long-term far infrared emission performance.
The invention further provides the following scheme: the elongation at break of the far infrared acrylic fiber is 40-48%, and the strength is 2.3-2.9 cN/dtex.
In the scheme, the initial elongation at break of the acrylic fiber serving as the base material is 42.0-48.0%, and the strength is 2.1-2.7 dcN/dtex. The far infrared component is introduced into the acrylic fiber in an in-situ polymerization mode, so that the far infrared component is uniformly distributed in the fiber, the basic mechanical property of the fiber is not affected, and the fiber is enhanced to a certain extent.
The invention also provides a preparation method of the far infrared acrylic fiber, which comprises the following steps:
(1) Mixing the far infrared component and polyethylene glycol and grinding and dispersing into far infrared slurry under ultrasonic conditions;
(2) Adding a reaction monomer into the far infrared slurry prepared in the step (1), and simultaneously adding a catalyst, an accelerator, an activator, an acid agent and a dispersing agent to enable the monomer to perform in-situ polymerization reaction between the far infrared nanometer molecular structure layers to prepare far infrared polymer slurry, and performing single removal, filtration and drying on the slurry to prepare the far infrared polymer;
(3) And (3) dissolving the far infrared polymer prepared in the step (2) in dimethylacetamide to obtain a glue solution, and carrying out wet solution spinning by taking the glue solution as a raw material to prepare the far infrared acrylic fiber.
In the scheme, in order to solve the problem of compatibility of the far infrared component and the acrylic fiber, the far infrared component is subjected to dispersion treatment in advance in the preparation process to obtain the far infrared slurry with a multi-void structure, so that a subsequent reaction monomer and a reaction reagent can enter voids of the slurry to form a reaction system, the acrylonitrile monomer is subjected to in-situ polymerization, and the generated polyacrylonitrile is deposited in the slurry along with the increase of the polymerization size to form a polymer uniformly dispersed with the far infrared component, thereby solving the problem that the far infrared component is easy to agglomerate, avoiding the situation that the far infrared component is too concentrated on the surface layer of the polymer, and enabling the spun fiber to have long far infrared emission performance.
According to the preparation method, the particle size of the far infrared slurry prepared in the step (1) is 0.1-10 mu m, and the solid content is 3.0-20.0wt%; preferably, the particle size of the far infrared slurry is 0.2-1 μm and the solid content is 5.0-15.0 wt%.
In the scheme, the far infrared component is ground and dispersed in polyethylene glycol according to a certain particle size range, and the addition amount of the polyethylene glycol is controlled, so that the slurry has a multi-void structure suitable for in-situ polymerization to uniformly occur.
According to the preparation method, the reaction temperature of the in-situ polymerization reaction in the step (2) is 55-65 ℃, the reaction time is 100-130 min, and the intrinsic viscosity of the prepared far infrared polymer slurry is 0.145-0.168 dL/g; preferably, the reaction temperature of the polymerization reaction is 59.0-60.0 ℃, the reaction time is 120min, and the intrinsic viscosity of the prepared far infrared polymer slurry is 0.150-0.156 dL/g.
According to the preparation method, the mass ratio of the far infrared component to the reaction monomer contained in the far infrared slurry in the step (2) is 2-5:100; the reaction monomer comprises acrylonitrile, vinyl acetate and sodium methacrylate sulfonate with the mass ratio of 12-14:1:0.2-0.8; the far infrared component is one or more selected from silicon oxide, aluminum oxide, sodium oxide, potassium oxide, calcium oxide, magnesium oxide, ferric oxide and titanium oxide; the far infrared component is preferably selected from ceramic powder with silicon oxide and aluminum oxide as main components, and also comprises a small amount of other components, wherein the other components are selected from one or more of sodium oxide, potassium oxide, calcium oxide, magnesium oxide, ferric oxide and titanium oxide.
In the above scheme, the mass requirements of the acrylonitrile are as follows: the color (Pt-Co) is not more than 10, the polymerization inhibitor is not more than 0.003-0.006%, the water is not more than 0.50%, the peroxide is not more than 0.00004%, the acetaldehyde is not more than 0.005%, and the acetone is not more than 0.01%.
According to the preparation method, the vacuum degree of the filtration in the step (2) is-20 to-40 kPa, the back flushing pressure is 200 to 600kPa, the mass flow rate of flushing water is 8000 to 15000kg/h, and the mass flow rate of spray water is 8000 to 15000kg/h; preferably, the vacuum degree is-25 to-35 kPa, the back flushing pressure is 300 to 400kPa, the mass flow rate of flushing water is 10000 to 13000kg/h, and the mass flow rate of spray water is 10000 to 14000kg/h.
According to the above preparation method, the drying in step (2) is performed by drying the filtered far infrared wet polymer slurry such that the water content of the far infrared polymer is reduced to 0.5 to 4.5wt%, preferably to 1.5 to 2.5wt%.
According to the preparation method, in the step (2), the catalyst is ammonium persulfate with the concentration of 1.0-4.0%, and the preferable concentration of the ammonium persulfate is 2.5-3.5%; the accelerator is ferrous sulfate with the concentration of 0.06-0.14%, and the preferable concentration of the ferrous sulfate is 0.08-0.12%; the acid agent is sulfuric acid with the concentration of 7-15%, and the preferential concentration of the sulfuric acid is 9-11%; the dispersant is desalted water with the pH value of 6.0-9.0, and the preferable pH value of the desalted water is 7.0-8.0; preferably, the mass ratio of the catalyst, the activator, the accelerator and the acid agent added into the reaction system is 28-30:5-5.5:0.7-0.9:1.
According to the preparation method, in the step (3), the content of the far infrared polymer in the glue solution is 24.0-26.0 wt%.
Specifically, the preparation method is used for preparing the far infrared acrylic fiber:
(1) Mixing and grinding the far infrared component and polyethylene glycol into far infrared slurry, wherein the particle size of the far infrared slurry is 0.1-10 mu m, and the solid content is 3.0-20.0 wt%;
(2) Mixing acrylonitrile, vinyl acetate and sodium methacrylate sulfonate with the mass ratio of 12-14:1:0.2-0.8 with far infrared slurry prepared in the step (1) at the mass ratio of 2-5:100, simultaneously adding a catalyst, an accelerator, an acid agent and a dispersing agent for polymerization reaction, wherein the reaction temperature is 55-65 ℃, the reaction time is 100-130 min, the intrinsic viscosity of the prepared far infrared polymer slurry is 0.145-0.168 dL/g, and the slurry is subjected to single removal, filtration and drying to prepare the far infrared polymer; the vacuum degree of the filtration is-20 to-40 kPa, the back flushing pressure is 200 to 600kPa, the mass flow rate of flushing water is 8000 to 15000kg/h, and the mass flow rate of spray water is 8000 to 15000kg/h; the drying is to dry the filtered far infrared wet polymer slurry so that the water content of the far infrared polymer is reduced to 0.5-4.5 wt%;
(3) Dissolving the far infrared polymer prepared in the step (2) in dimethylacetamide to obtain a glue solution with the content of the far infrared polymer of 24.0-26.0 wt%, and carrying out wet spinning by taking the glue solution as a raw material to prepare the far infrared acrylic fiber.
After the technical scheme is adopted, compared with the prior art, the invention has the following beneficial effects:
1. the preparation method of the far infrared acrylic fiber adopts an in-situ polymerization mode, so that the problem that far infrared components are easy to agglomerate is solved, the situation that the far infrared components are too concentrated on the surface layer of the polymer is avoided, and the spun fiber has long-term far infrared emission performance;
2. in the preparation method of the far infrared acrylic fiber, the far infrared component is subjected to dispersion treatment in advance in the preparation process to obtain the far infrared slurry with a multi-void structure, so that the subsequent reaction monomer and the reaction reagent can enter voids of the slurry to form a reaction system, the acrylonitrile monomer can be subjected to uniform in-situ polymerization, and the compatibility of the far infrared component and the fiber component is improved.
3. The far infrared acrylic fiber provided by the invention introduces far infrared components in an in-situ polymerization mode, and changes the molecular structure of the polymer on the premise of keeping the characteristics of the acrylic fiber, so that the fiber has a continuous electromagnetic wave emission function and good stability.
The following describes the embodiments of the present invention in further detail with reference to the accompanying drawings.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention. It is evident that the drawings in the following description are only examples, from which other drawings can be obtained by a person skilled in the art without the inventive effort. In the drawings:
FIG. 1 is a microscopic view of a far-infrared slurry having a solids content of 8.0wt% in example 1 of the present invention;
FIG. 2 is a microscopic view of a far-infrared slurry having a solids content of 15.0wt% in example 2 of the present invention;
FIG. 3 is a microscopic view of far-infrared slurry having a solid content of 10.0wt% in example 3 of the present invention.
It should be noted that these drawings and the written description are not intended to limit the scope of the inventive concept in any way, but to illustrate the inventive concept to those skilled in the art by referring to the specific embodiments.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments will be clearly and completely described with reference to the accompanying drawings in the embodiments of the present invention, and the following embodiments are used to illustrate the present invention, but are not intended to limit the scope of the present invention.
Example 1
In this example, acrylic fibers were prepared by the following method:
(1) Mixing the far infrared component and polyethylene glycol, and grinding and dispersing into far infrared slurry under ultrasonic condition, wherein the particle size of the far infrared slurry is 1 μm, and the solid content is 8.0wt%;
(2) Mixing acrylonitrile, vinyl acetate and sodium methyl propylene sulfonate with the mass ratio of 12.45:1:0.25 with the far infrared slurry prepared in the step (1) to obtain a mixture with the mass ratio of 2:100, and simultaneously adding a catalyst ammonium persulfate with the preparation concentration of 4%, an activator sodium bisulfite with the preparation concentration of 22%, an accelerator ferrous sulfate with the preparation concentration of 0.12%, an acid agent sulfuric acid with the preparation concentration of 11% and a dispersant desalted water with the pH of 8.0 for polymerization, wherein the mass ratio of the added catalyst, the activator, the accelerator and the acid agent is 28.1:5.2:0.78:1: the reaction temperature is 60.5 ℃, the reaction time is 120min, the intrinsic viscosity of the prepared far infrared polymer slurry is 0.160-0.167 dL/g, and the slurry is subjected to single removal, filtration and drying to prepare the far infrared polymer; the vacuum degree of the filtration is-35 kPa, the back flushing pressure is 400kPa, the mass flow rate of flushing water is 13000kg/h, and the mass flow rate of spray water is 14000kg/h; the drying is to dry the filtered far infrared wet polymer slurry so that the water content of the far infrared polymer is reduced to 0.5wt%;
(3) Dissolving the far infrared polymer prepared in the step (2) in dimethylacetamide to obtain a glue solution with the content of the far infrared polymer of 24.0wt%, and carrying out wet spinning with the glue solution as a raw material and the shaping pressure of 320kPa to prepare the far infrared acrylic fiber.
Example 2
In this example, acrylic fibers were prepared by the following method:
(1) Mixing the far infrared component and polyethylene glycol, and grinding and dispersing into far infrared slurry under ultrasonic condition, wherein the particle size of the far infrared slurry is 1 μm, and the solid content is 15.0wt%;
(2) Mixing acrylonitrile, vinyl acetate and sodium methyl propylene sulfonate with the mass ratio of 13.88:1:0.69 with the far infrared slurry prepared in the step (1) to obtain a mixture with the mass ratio of 5:100, and simultaneously adding a catalyst ammonium persulfate with the preparation concentration of 1%, an activator sodium bisulfite with the preparation concentration of 17%, an accelerator ferrous sulfate with the preparation concentration of 0.06%, an acid sulfuric acid with the preparation concentration of 9% and a dispersant desalted water with the pH of 9.0 for polymerization, wherein the mass ratio of the added catalyst to the activator to the accelerator to the acid is 30:5.5:0.8:1: the reaction temperature is 58.5 ℃, the reaction time is 120min, the intrinsic viscosity of the prepared far infrared polymer slurry is 0.158-0.163 dL/g, and the slurry is subjected to single removal, filtration and drying to prepare the far infrared polymer; the vacuum degree of the filtration is-25 kPa, the back flushing pressure is 600kPa, the mass flow rate of flushing water is 8000kg/h, and the mass flow rate of spray water is 10000kg/h; the drying is to dry the filtered far infrared wet polymer slurry so that the water content of the far infrared polymer is reduced to 4.5wt%;
(3) Dissolving the far infrared polymer prepared in the step (2) in dimethylacetamide to obtain a glue solution with the content of the far infrared polymer of 25.0wt%, and carrying out wet spinning with the glue solution as a raw material and the shaping pressure of 320kPa to prepare the far infrared acrylic fiber.
Example 3
In this example, acrylic fibers were prepared by the following method:
(1) Mixing the far infrared component and polyethylene glycol, and grinding and dispersing into far infrared slurry under ultrasonic condition, wherein the particle size of the far infrared slurry is 1 mu m, and the solid content is 10.0wt%;
(2) Mixing acrylonitrile, vinyl acetate and sodium methyl propylene sulfonate with the mass ratio of 13.26:1:0.38 with the far infrared slurry prepared in the step (1) to obtain a mixture with the mass ratio of 3:100, and simultaneously adding a catalyst ammonium persulfate with the preparation concentration of 3.5%, an activator sodium bisulfite with the preparation concentration of 25%, an accelerator ferrous sulfate with the preparation concentration of 0.08%, an acid sulfuric acid with the preparation concentration of 7% and a dispersant desalted water with the pH of 7.0 for polymerization, wherein the mass ratio of the catalyst, the activator, the accelerator and the acid is 29.3:5.3:0.9:1: the reaction temperature is 59 ℃, the reaction time is 120min, the intrinsic viscosity of the prepared far infrared polymer slurry is 0.153-0.156 dL/g, and the slurry is subjected to single removal, filtration and drying to prepare the far infrared polymer; the vacuum degree of the filtration is-20 kPa, the back flushing pressure is 300kPa, the mass flow rate of flushing water is 15000kg/h, and the mass flow rate of spray water is 15000kg/h; the drying is to dry the filtered far infrared wet polymer slurry so that the water content of the far infrared polymer is reduced to 2.5wt%;
(3) Dissolving the far infrared polymer prepared in the step (2) in dimethylacetamide to obtain a glue solution with the content of the far infrared polymer of 26.0wt%, and spinning the glue solution by a wet method with the sizing pressure of 320kPa serving as a raw material to prepare the far infrared acrylic fiber.
Example 4
In this example, acrylic fibers were prepared by the following method:
(1) Mixing the far infrared component and polyethylene glycol, and grinding and dispersing into far infrared slurry under ultrasonic condition, wherein the particle size of the far infrared slurry is 0.2 mu m, and the solid content is 20wt%;
(2) Mixing acrylonitrile, vinyl acetate and sodium methyl propylene sulfonate with the mass ratio of 12.45:1:0.25 with the far infrared slurry prepared in the step (1) to obtain a mixture with the mass ratio of 4:100, and simultaneously adding a catalyst ammonium persulfate with the preparation concentration of 2.5%, an activator sodium bisulfite with the preparation concentration of 15%, an accelerator ferrous sulfate with the preparation concentration of 0.14%, an acid sulfuric acid with the preparation concentration of 15% and a dispersant desalted water with the pH of 6.0 for polymerization, wherein the mass ratio of the catalyst, the activator, the accelerator and the acid is 28.1:5.2:0.78:1: the reaction temperature is 65 ℃ and the reaction time is 100min, the intrinsic viscosity of the prepared far infrared polymer slurry is 0.145-0.15 dL/g, and the slurry is subjected to single removal, filtration and drying to prepare the far infrared polymer; the vacuum degree of the filtration is-40 kPa, the back flushing pressure is 200kPa, the mass flow rate of flushing water is 10000kg/h, and the mass flow rate of spray water is 8000kg/h; the drying is to dry the filtered far infrared wet polymer slurry so that the water content of the far infrared polymer is reduced to 1.5wt%;
(3) Dissolving the far infrared polymer prepared in the step (2) in dimethylacetamide to obtain a glue solution with the content of the far infrared polymer of 24.0wt%, and carrying out wet spinning with the glue solution as a raw material and the shaping pressure of 320kPa to prepare the far infrared acrylic fiber.
Example 5
In this example, acrylic fibers were prepared by the following method:
(1) Mixing the far infrared component and polyethylene glycol, and grinding and dispersing into far infrared slurry under ultrasonic condition, wherein the particle size of the far infrared slurry is 10 mu m, and the solid content is 3wt%;
(2) Mixing acrylonitrile, vinyl acetate and sodium methyl propylene sulfonate with the mass ratio of 13.88:1:0.69 with the far infrared slurry prepared in the step (1) to obtain a mixture with the mass ratio of 2:100, and simultaneously adding a catalyst ammonium persulfate with the preparation concentration of 3%, an activator sodium bisulfite with the preparation concentration of 20%, an accelerator ferrous sulfate with the preparation concentration of 0.1%, an acid sulfuric acid with the preparation concentration of 10% and a dispersant desalted water with the pH of 7.5 for polymerization, wherein the mass ratio of the added catalyst to the activator to the accelerator to the acid is 30:5.5:0.8:1: the reaction temperature is 55 ℃, the reaction time is 130min, the intrinsic viscosity of the prepared far infrared polymer slurry is 0.16-0.168 dL/g, and the slurry is subjected to single removal, filtration and drying to prepare the far infrared polymer; the vacuum degree of the filtration is-30 kPa, the back flushing pressure is 360kPa, the mass flow rate of flushing water is 12000kg/h, and the mass flow rate of spray water is 12500kg/h; the drying is to dry the filtered far infrared wet polymer slurry so that the water content of the far infrared polymer is reduced to 2.2wt%;
(3) Dissolving the far infrared polymer prepared in the step (2) in dimethylacetamide to obtain a glue solution with the content of the far infrared polymer of 25.0wt%, and carrying out wet spinning with the glue solution as a raw material and the shaping pressure of 320kPa to prepare the far infrared acrylic fiber.
Example 6
In this example, acrylic fibers were prepared by the following method:
(1) Mixing the far infrared component and polyethylene glycol, and grinding and dispersing into far infrared slurry under ultrasonic condition, wherein the particle size of the far infrared slurry is 0.1 mu m, and the solid content is 5wt%;
(2) Mixing acrylonitrile, vinyl acetate and sodium methyl propylene sulfonate with the mass ratio of 13.26:1:0.38 with the far infrared slurry prepared in the step (1) to obtain a mixture with the mass ratio of 3:100, and simultaneously adding a catalyst ammonium persulfate with the preparation concentration of 3.5%, an activator sodium bisulfite with the preparation concentration of 25%, an accelerator ferrous sulfate with the preparation concentration of 0.08%, an acid sulfuric acid with the preparation concentration of 7% and a dispersant desalted water with the pH of 7.0 for polymerization, wherein the mass ratio of the catalyst, the activator, the accelerator and the acid is 29.3:5.3:0.9:1: the reaction temperature is 59 ℃, the reaction time is 120min, the intrinsic viscosity of the prepared far infrared polymer slurry is 0.154-0.158 dL/g, and the slurry is subjected to single removal, filtration and drying to prepare the far infrared polymer; the vacuum degree of the filtration is-36 kPa, the back flushing pressure is 500kPa, the mass flow rate of flushing water is 9000kg/h, and the mass flow rate of spray water is 14500kg/h; the drying is to dry the filtered far infrared wet polymer slurry so that the water content of the far infrared polymer is reduced to 1.2wt%;
(3) Dissolving the far infrared polymer prepared in the step (2) in dimethylacetamide to obtain a glue solution with the content of the far infrared polymer of 26.0wt%, and carrying out wet spinning with the glue solution as a raw material and the shaping pressure of 320kPa to prepare the far infrared acrylic fiber.
Comparative examples 1 to 3
Comparative examples 1 to 3 acrylic fibers were prepared without adding a far infrared component based on examples 1 to 3, respectively, and other embodiments of comparative examples 1 to 3 were the same as examples 1 to 3.
Experimental example 1
In this experimental example, the intrinsic viscosity and vinyl acetate content of the far infrared polymers prepared in step (2) in examples 1 to 6 were measured, respectively, and the results are shown in table 1; the far infrared acrylic fibers prepared in examples 1 to 6 and comparative examples 1 to 3 were then analyzed and tested, and the results are shown in Table 2, below in detail:
TABLE 1 far infrared Polymer test data sheet
| Polymer extra-viscous (dL/g) | Vinyl acetate content (%) | |
| Example 1 | 0.163 | 6.02 |
| Example 2 | 0.161 | 5.52 |
| Example 3 | 0.157 | 5.95 |
| Example 4 | 0.166 | 6.13 |
| Example 5 | 0.163 | 5.63 |
| Example 6 | 0.160 | 5.99 |
TABLE 2 full analysis results of far infrared fibers
As can be seen from the above table, the far infrared acrylic fibers prepared in examples 1 to 6 have higher emissivity in the range of the optimal infrared absorption wavelength of the human body, while the acrylic fibers prepared by removing the far infrared component based on examples 1 to 3 and comparing the elongation at break and the strength parameter, the far infrared component is introduced into the acrylic fibers by the in-situ polymerization method, so that the far infrared component is uniformly distributed in the fibers, the basic mechanical properties of the fibers are not affected, and the fibers are enhanced to a certain extent.
The foregoing description is only illustrative of the preferred embodiment of the present invention, and is not to be construed as limiting the invention, but is to be construed as limiting the invention to any and all simple modifications, equivalent variations and adaptations of the embodiments described above, which are within the scope of the invention, may be made by those skilled in the art without departing from the scope of the invention.
Claims (15)
1. The far infrared acrylic fiber is characterized in that the emissivity of the far infrared acrylic fiber at the wavelength of 4-14 mu m is 0.82-0.89; the elongation at break of the far infrared acrylic fiber is 40-48%;
the far infrared acrylic fiber is prepared by the following preparation method:
(1) Mixing the far infrared component and polyethylene glycol and grinding and dispersing into far infrared slurry under ultrasonic conditions; the particle size of the far infrared slurry is 0.1-10 mu m, and the solid content is 3.0-20.0wt%; the far infrared component is one or more selected from silicon oxide, aluminum oxide, sodium oxide, potassium oxide, calcium oxide, magnesium oxide, ferric oxide and titanium oxide;
(2) Adding a reaction monomer into the far infrared slurry prepared in the step (1), and simultaneously adding a catalyst, an accelerator, an activator, an acid agent and a dispersing agent to enable the monomer to perform in-situ polymerization reaction between the far infrared nanometer molecular structure layers to prepare far infrared polymer slurry, and performing single removal, filtration and drying on the slurry to prepare the far infrared polymer; the mass ratio of the far infrared component to the reaction monomer contained in the far infrared slurry is 2-5:100; the reaction monomer comprises acrylonitrile, vinyl acetate and sodium methacrylate sulfonate with the mass ratio of 12-14:1:0.2-0.8; the catalyst is ammonium persulfate with the preparation concentration of 1.0-4.0%, the activator is sodium bisulphite with the preparation concentration of 15.0-25.0%, the promoter is ferrous sulfate with the preparation concentration of 0.06-0.14%, the acid agent is sulfuric acid with the preparation concentration of 7-15%, and the dispersing agent is desalted water with the pH value of 6.0-9.0;
(3) And (3) dissolving the far infrared polymer prepared in the step (2) in dimethylacetamide to obtain a glue solution, and carrying out wet solution spinning by taking the glue solution as a raw material to prepare the far infrared acrylic fiber.
2. The far infrared acrylic fiber according to claim 1, wherein the far infrared acrylic fiber has a strength of 2.3 to 2.9cN/dtex.
3. A method for producing the far infrared acrylic fiber according to claim 1 or 2, comprising:
(1) Mixing the far infrared component and polyethylene glycol and grinding and dispersing into far infrared slurry under ultrasonic conditions;
(2) Adding a reaction monomer into the far infrared slurry prepared in the step (1), and simultaneously adding a catalyst, an accelerator, an activator, an acid agent and a dispersing agent to enable the monomer to perform in-situ polymerization reaction between the far infrared nanometer molecular structure layers to prepare far infrared polymer slurry, and performing single removal, filtration and drying on the slurry to prepare the far infrared polymer;
(3) And (3) dissolving the far infrared polymer prepared in the step (2) in dimethylacetamide to obtain a glue solution, and carrying out wet solution spinning by taking the glue solution as a raw material to prepare the far infrared acrylic fiber.
4. The method for preparing far infrared acrylic fiber according to claim 3, wherein the particle size of the far infrared slurry prepared in the step (1) is 0.1-10 μm, and the solid content is 3.0-20.0 wt%.
5. The method for producing far infrared acrylic fiber according to claim 4, wherein the particle size of the far infrared slurry is 0.2 to 1 μm and the solid content is 5.0 to 15.0wt%.
6. The method for preparing far infrared acrylic fiber according to claim 3, wherein the reaction temperature of the in-situ polymerization in the step (2) is 55-65 ℃ and the reaction time is 100-130 min, and the intrinsic viscosity of the prepared far infrared polymer slurry is 0.145-0.168 dL/g.
7. The method for producing far infrared acrylic fiber according to claim 6, wherein the polymerization reaction is carried out at a reaction temperature of 59.0 to 60.0 ℃ for 120 minutes, and the resulting far infrared polymer slurry has an intrinsic viscosity of 0.150 to 0.156dL/g.
8. The method for producing far-infrared acrylic fiber according to claim 3, wherein the far-infrared component is one or more selected from the group consisting of silica, alumina, sodium oxide, potassium oxide, calcium oxide, magnesium oxide, iron oxide, and titanium oxide.
9. The method for producing far infrared acrylic fiber according to claim 3, wherein the vacuum degree of the filtration in the step (2) is-20 to-40 kPa, the back blowing pressure is 200 to 600kPa, and the mass flow rate of flushing water is 8000 to 15000kg/h; the mass flow rate of the spray water is 8000-15000 kg/h.
10. The method for producing far infrared acrylic fiber according to claim 9, wherein in the step (2), the vacuum degree is-25 to-35 kPa, the back blowing pressure is 300 to 400kPa, the mass flow rate of flushing water is 10000 to 13000kg/h, and the mass flow rate of shower water is 10000 to 14000kg/h.
11. A process for the preparation of far infrared acrylic fiber according to claim 3, wherein the drying in step (2) is drying the filtered far infrared wet polymer slurry such that the water content of the far infrared polymer is reduced to 0.5 to 4.5wt%.
12. The method for producing far infrared acrylic fiber according to claim 11, wherein the water content of the far infrared polymer in the step (2) is reduced to 1.5 to 2.5wt%.
13. The method for producing far-infrared acrylic fiber according to claim 3, wherein in the step (2), the concentration of the ammonium persulfate is 2.5 to 3.5%; the preparation concentration of the sodium bisulphite is 17-22%; the preparation concentration of the ferrous sulfate is 0.08-0.12%; the concentration of the sulfuric acid is 9-11%; the pH value of the desalted water is 7.0-8.0.
14. The method for preparing far infrared acrylic fiber according to claim 13, wherein the mass ratio of the catalyst, the activator, the accelerator and the acid agent added into the reaction system is 28-30:5-5.5:0.7-0.9:1.
15. The method for producing far infrared acrylic fiber according to claim 3, wherein in the step (3), the content of the far infrared polymer in the dope is 24.0 to 26.0wt%.
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