CN112127000A - Far infrared acrylic fiber and preparation method thereof - Google Patents
Far infrared acrylic fiber and preparation method thereof Download PDFInfo
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- CN112127000A CN112127000A CN202010919616.4A CN202010919616A CN112127000A CN 112127000 A CN112127000 A CN 112127000A CN 202010919616 A CN202010919616 A CN 202010919616A CN 112127000 A CN112127000 A CN 112127000A
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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 far infrared acrylic fiber and a preparation method thereof, wherein the specific radiance 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 under ultrasonic condition to obtain far infrared slurry; (2) adding a reaction monomer into the far infrared slurry, simultaneously adding a catalyst, an accelerant, an activating agent, an acid agent and a dispersing agent, carrying out in-situ polymerization reaction on the monomer between layers of the far infrared nano molecular structure to prepare far infrared polymer slurry, and then carrying out demonomerization, filtration and drying on the slurry to prepare a far infrared polymer; (3) and dissolving the far infrared polymer in dimethylacetamide to obtain a glue solution, and performing wet solution spinning to obtain the far infrared acrylic fiber. The invention adopts an in-situ polymerization mode and a wet two-step acrylic fiber process method to prepare the far infrared acrylic fiber so as to ensure that the product has long-term 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 far infrared acrylic fibers and a preparation method thereof.
Background
Along with the improvement of life quality of people, the demand of functional fiber products is rapidly improved, and the far infrared acrylic fiber is novel functional fiber with the functions of absorbing and emitting far infrared electromagnetic waves. The acrylic fiber compounded with the nano inorganic far infrared health-care components can emit high and far infrared electromagnetic waves with wavelengths 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, and can effectively improve human body microcirculation, improve oxygen supply of tissues, activate tissue cells, improve metabolism, prevent aging, strengthen immune systems and the like. The far infrared acrylic fiber also has excellent mothproof property and good fluffy feeling and comfortable feeling, has hand feeling similar to wool, and has wearing comfort and air permeability which meet the requirements 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 current preparation method of far infrared functional acrylic fiber is a solution blending spinning method in the processes of stock solution glue making and spinning, namely, a far infrared fiber is prepared by blending and melting spinning method of ceramic particles with far infrared radiation function and conventional polymers; the method can also be used for post-treatment of the coating of the forming fabric, and the mode is that far infrared nanometer powder is mixed in the fiber and the coating realizes the far infrared function, so that the produced far infrared acrylic fiber only macroscopically increases the far infrared components, and the uniformity and the stability of the far infrared function of the fiber have defects, so that the far infrared acrylic fiber textile product prepared by the method can also weaken the far infrared function to some extent in the using process, thereby reducing the far infrared emissivity and the far infrared effect.
Compared with the solution blending spinning method for manufacturing far infrared acrylic fiber, the method has the advantages that the molecular structure of polyacrylonitrile polymer used for producing acrylic fiber is changed by an in-situ polymerization method, so that the aim that the far infrared acrylic fiber produced by a wet process has the function of continuous electromagnetic wave emission is fulfilled.
The research and development of far infrared technology at normal temperature in Japan is at the international leading level, according to the introduction 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. The in-situ polymerization reaction can realize the modification of the molecular structure of the polymer by adding nanometer material components. Because the in-situ polymerization reaction is complex, the requirements on the particle size of the added ceramic powder with the far infrared function and the selection technology of the dispersing agent are high, otherwise, the spinning difficulty is caused to influence the fiber quality, and the agglomeration occurs after the dispersion to influence the progress of the polymerization reaction. At present, the technical data and reports of the in-situ polymerization reaction used for the acrylic fiber are few, and the laboratory research is limited, and no comparative system, mature research data and market production example exists.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides far infrared acrylic fiber and a preparation method thereof, wherein the preparation method comprises the steps of dispersing a far infrared component in advance to form a far infrared slurry with a plurality of gaps among molecules, so that a reaction monomer and a reaction reagent which are added subsequently form an oxidation-reduction system in the far infrared slurry to complete the subsequent in-situ polymerization reaction, and the product has long-term far infrared emission performance and better mechanical stability.
In order to solve the technical problems, the invention adopts the technical scheme that:
the invention provides far infrared acrylic fibers, which have the specific radiance of 0.82-0.89 at the wavelength of 4-14 mu m.
In the scheme, the far infrared acrylic fiber has higher specific radiance in the range of the optimal infrared absorption wavelength of a human body. Because adopt the in situ polymerization mode to introduce acrylic fiber with far infrared component, compare among the prior art with the direct addition of far infrared component in acrylic fiber spinning solution, or compare at the scheme that the fibre surface was coated, the acrylic fiber that this application provided has permanent far infrared emission performance.
The further scheme of the invention is as follows: 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 above aspect, the acrylic fiber as the base material has an initial elongation at break of 42.0 to 48.0% and a strength of 2.1 to 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 influenced, 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 under ultrasonic condition to obtain far infrared slurry;
(2) adding a reaction monomer into the far infrared slurry prepared in the step (1), and simultaneously adding a catalyst, an accelerant, an activating agent, an acid agent and a dispersing agent to enable the monomer to generate in-situ polymerization reaction between the layers of the far infrared nano molecular structure to prepare far infrared polymer slurry, and then removing the monomer, filtering and drying the slurry to prepare a far infrared polymer;
(3) and (3) dissolving the far infrared polymer prepared in the step (2) in dimethylacetamide to obtain a glue solution, and performing wet solution spinning by taking the glue solution as a raw material to obtain 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-gap structure, so that subsequent reaction monomers and reaction reagents can enter gaps of the slurry to form a reaction system, acrylonitrile monomers are subjected to in-situ polymerization, and the generated polyacrylonitrile is deposited in the slurry along with the increase of polymerization size to form a polymer with the uniformly dispersed far infrared component, so that the problem of easy agglomeration of the far infrared component is solved, the situation that the far infrared component is excessively concentrated on the surface layer of the polymer is also avoided, and the spun fiber has long-term 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 3.0-20.0 wt%; 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 above scheme, the present invention grinds and disperses the far infrared component in polyethylene glycol according to a certain particle size range, while controlling the addition amount of polyethylene glycol, so that the slurry has a porous structure suitable for uniform occurrence of in-situ polymerization.
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 components contained in the far infrared slurry in the step (2) to the reaction monomers is 2-5: 100; the reaction monomer comprises acrylonitrile, vinyl acetate and sodium methyl propylene sulfonate in a mass ratio of 12-14: 1: 0.2-0.8; the far infrared component is selected from one or more of silicon oxide, aluminum oxide, sodium oxide, potassium oxide, calcium oxide, magnesium oxide, iron oxide and titanium oxide; preferably, the far infrared component is selected from ceramic powder taking 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, iron oxide and titanium oxide.
In the scheme, the acrylonitrile has the following quality requirements: chroma (Pt-Co) is not more than 10, polymerization inhibitor content is not more than 0.003-0.006%, moisture is not more than 0.50%, peroxide content is not more than 0.00004%, acetaldehyde content is not more than 0.005%, and acetone content 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 of the flushing water is 8000 to 15000kg/h, and the mass flow of the spray water is 8000 to 15000 kg/h; preferably, the vacuum degree is-25 to-35 kPa, the back flushing pressure is 300 to 400kPa, the mass flow of flushing water is 10000 to 13000kg/h, and the mass flow of shower water is 10000 to 14000 kg/h.
According to the above preparation method, the drying in the step (2) is drying the filtered far infrared wet polymer slurry to reduce the water content of the far infrared polymer to 0.5 to 4.5 wt%, preferably to 1.5 to 2.5 wt%.
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 preferable concentration of the sulfuric acid is 9-11%; the dispersing agent 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 activating agent, the promoter 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 far infrared acrylic fiber is prepared by the following preparation method:
(1) mixing and grinding far infrared components 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 methallylsulfonate with the far infrared slurry prepared in the step (1) in a mass ratio of 12-14: 1: 0.2-0.8, mixing the mixture in a mass ratio of 2-5: 100, adding a catalyst, an accelerator, an acid agent and a dispersing agent for polymerization reaction at a reaction temperature of 55-65 ℃ for 100-130 min, wherein the intrinsic viscosity of the prepared far infrared polymer slurry is 0.145-0.168 dL/g, and performing demonomerization, filtration and drying on the slurry to prepare a 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 of flushing water is 8000 to 15000kg/h, and the mass flow of spray water is 8000 to 15000 kg/h; the drying is to dry the filtered far infrared wet polymer slurry to reduce the water content of the far infrared polymer to 0.5-4.5 wt%;
(3) and (3) dissolving the far infrared polymer prepared in the step (2) in dimethylacetamide to obtain glue solution with the content of the far infrared polymer of 24.0-26.0 wt%, and performing wet spinning by taking the glue solution as a raw material to obtain the far infrared acrylic fiber.
After adopting the technical scheme, compared with the prior art, the invention has the following beneficial effects:
1. the preparation method of the far infrared acrylic fiber provided by the invention adopts an in-situ polymerization mode, not only solves the problem that far infrared components are easy to agglomerate, but also avoids the situation that the far infrared components are excessively concentrated on the surface layer of a polymer, so that the spun fiber has long-term far infrared emission performance;
2. in the preparation method of the far infrared acrylic fiber provided by the invention, the far infrared component is dispersed in advance in the preparation process to obtain the far infrared slurry with a multi-gap structure, so that subsequent reaction monomers and reaction reagents can enter gaps of the slurry to form a reaction system, the acrylonitrile monomers can be subjected to uniform in-situ polymerization reaction, and the compatibility of the far infrared component and the fiber component is improved.
3. The far infrared acrylic fiber provided by the invention adopts an in-situ polymerization mode to introduce far infrared components, changes the molecular structure of the polymer on the premise of keeping the characteristics of the acrylic fiber, and ensures that the fiber has a continuous electromagnetic wave emission function and good stability.
The following describes 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, 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 without limiting the invention to the right. It is obvious that the drawings in the following description are only some embodiments, and that for a person skilled in the art, other drawings can be derived from them without inventive effort. In the drawings:
FIG. 1 is a microscopic observation view of far infrared slurry having a solid content of 8.0 wt% in example 1 of the present invention;
FIG. 2 is a microscopic observation view of far infrared slurry having a solid content of 15.0 wt% in example 2 of the present invention;
FIG. 3 is a microscopic observation view of far infrared slurry having a solid content of 10.0 wt% in example 3 of the present invention.
It should be noted that the drawings and the description are not intended to limit the scope of the inventive concept in any way, but to illustrate it by a person skilled in the art with reference to specific embodiments.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and the following embodiments are used for illustrating the present invention and are not intended to limit the scope of the present invention.
Example 1
In this example, the acrylic fiber was prepared by the following method:
(1) mixing far infrared component and polyethylene glycol, and grinding and dispersing under ultrasonic condition to obtain far infrared slurry with particle diameter of 1 μm and solid content of 8.0 wt%;
(2) mixing acrylonitrile, vinyl acetate and sodium methallyl sulfonate in a mass ratio of 12.45:1:0.25 with the far infrared slurry prepared in the step (1) in a mass ratio of 2:100, simultaneously adding a catalyst ammonium persulfate with a preparation concentration of 4%, an activator sodium bisulfite with a preparation concentration of 22%, an accelerator ferrous sulfate with a preparation concentration of 0.12%, an acid agent sulfuric acid with a preparation concentration of 11% and a dispersant desalted water with a pH value of 8.0 for polymerization, adding a catalyst, an activator, an accelerator and an acid agent in a mass ratio of 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 demonomerization, 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 of flushing water is 13000kg/h, and the mass flow of spray water is 14000 kg/h; the drying is to dry the filtered far infrared wet polymer slurry to reduce the water content of the far infrared polymer to 0.5 wt%;
(3) and (3) dissolving the far infrared polymer prepared in the step (2) in dimethylacetamide to obtain glue solution with the content of the far infrared polymer being 24.0 wt%, and performing wet spinning with the glue solution as a raw material and the setting pressure being 320kPa to obtain the far infrared acrylic fiber.
Example 2
In this example, the acrylic fiber was prepared by the following method:
(1) mixing far infrared component and polyethylene glycol, and grinding and dispersing under ultrasonic condition to obtain far infrared slurry with particle diameter of 1 μm and solid content of 15.0 wt%;
(2) mixing acrylonitrile, vinyl acetate and sodium methallyl sulfonate in a mass ratio of 13.88:1:0.69 with the far infrared slurry prepared in the step (1) in a mass ratio of 5:100, simultaneously adding a catalyst ammonium persulfate with a preparation concentration of 1%, an activator sodium bisulfite with a preparation concentration of 17%, an accelerator ferrous sulfate with a preparation concentration of 0.06%, an acid agent sulfuric acid with a preparation concentration of 9% and a dispersant desalted water with a pH value of 9.0 for polymerization, adding a catalyst, an activator, an accelerator and an acid agent in a mass ratio of 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 demonomerization, 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 of flushing water is 8000kg/h, and the mass flow of spray water is 10000 kg/h; the drying is to dry the filtered far infrared wet polymer slurry to reduce the water content of the far infrared polymer to 4.5 wt%;
(3) and (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 being 25.0 wt%, and performing wet spinning with the glue solution as a raw material and the setting pressure being 320kPa to obtain the far infrared acrylic fiber.
Example 3
In this example, the acrylic fiber was prepared by the following method:
(1) mixing far infrared component and polyethylene glycol, and grinding and dispersing under ultrasonic condition to obtain far infrared slurry with particle diameter of 1 μm and solid content of 10.0 wt%;
(2) mixing acrylonitrile, vinyl acetate and sodium methallyl sulfonate in a mass ratio of 13.26:1:0.38 with the far infrared slurry prepared in the step (1) in a mass ratio of 3:100, simultaneously adding a catalyst ammonium persulfate with a preparation concentration of 3.5%, an activator sodium bisulfite with a preparation concentration of 25%, an accelerator ferrous sulfate with a preparation concentration of 0.08%, an acid agent sulfuric acid with a preparation concentration of 7% and a dispersant desalted water with a pH value of 7.0 for polymerization, adding a catalyst, an activator, an accelerator and an acid agent in a mass ratio of 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 separation, filtration and drying to prepare a far infrared polymer; the vacuum degree of the filtration is-20 kPa, the back flushing pressure is 300kPa, the mass flow of flushing water is 15000kg/h, and the mass flow of spray water is 15000 kg/h; the drying is to dry the filtered far infrared wet polymer slurry to reduce the water content of the far infrared polymer to 2.5 wt%;
(3) and (3) dissolving the far infrared polymer prepared in the step (2) in dimethylacetamide to obtain a glue solution with the far infrared polymer content of 26.0 wt%, and performing wet spinning by taking the glue solution as a raw material under the shaping pressure of 320kPa to obtain the far infrared acrylic fiber.
Example 4
In this example, the acrylic fiber was prepared by the following method:
(1) mixing far infrared component and polyethylene glycol, and grinding and dispersing under ultrasonic condition to obtain far infrared slurry with particle diameter of 0.2 μm and solid content of 20 wt%;
(2) mixing acrylonitrile, vinyl acetate and sodium methallyl sulfonate in a mass ratio of 12.45:1:0.25 with the far infrared slurry prepared in the step (1) in a mass ratio of 4:100, simultaneously adding a catalyst ammonium persulfate with a preparation concentration of 2.5%, an activator sodium bisulfite with a preparation concentration of 15%, an accelerator ferrous sulfate with a preparation concentration of 0.14%, an acid agent sulfuric acid with a preparation concentration of 15% and a dispersant desalted water with a pH value of 6.0 for polymerization, adding a catalyst, an activator, an accelerator and an acid agent in a mass ratio of 28.1:5.2:0.78: 1: the reaction temperature is 65 ℃, 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 separation, filtration and drying to prepare a far infrared polymer; the vacuum degree of the filtration is-40 kPa, the back flushing pressure is 200kPa, the mass flow of flushing water is 10000kg/h, and the mass flow of spray water is 8000 kg/h; the drying is to dry the filtered far infrared wet polymer slurry to reduce the water content of the far infrared polymer to 1.5 wt%;
(3) and (3) dissolving the far infrared polymer prepared in the step (2) in dimethylacetamide to obtain glue solution with the content of the far infrared polymer being 24.0 wt%, and performing wet spinning with the glue solution as a raw material and the setting pressure being 320kPa to obtain the far infrared acrylic fiber.
Example 5
In this example, the acrylic fiber was prepared by the following method:
(1) mixing far infrared component and polyethylene glycol, and grinding and dispersing under ultrasonic condition to obtain far infrared slurry with particle diameter of 10 μm and solid content of 3 wt%;
(2) mixing acrylonitrile, vinyl acetate and sodium methallyl sulfonate in a mass ratio of 13.88:1:0.69 with the far infrared slurry prepared in the step (1) in a mass ratio of 2:100, simultaneously adding a catalyst ammonium persulfate with a preparation concentration of 3%, an activator sodium bisulfite with a preparation concentration of 20%, an accelerator ferrous sulfate with a preparation concentration of 0.1%, an acid agent sulfuric acid with a preparation concentration of 10% and a dispersant desalted water with a pH value of 7.5 for polymerization, adding a catalyst, an activator, an accelerator and an acid agent in a mass ratio of 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 separation, filtration and drying to prepare a far infrared polymer; the vacuum degree of the filtration is-30 kPa, the back flushing pressure is 360kPa, the mass flow of flushing water is 12000kg/h, and the mass flow of spray water is 12500 kg/h; the drying is to dry the filtered far infrared wet polymer slurry to reduce the water content of the far infrared polymer to 2.2 wt%;
(3) and (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 being 25.0 wt%, and performing wet spinning with the glue solution as a raw material and the setting pressure being 320kPa to obtain the far infrared acrylic fiber.
Example 6
In this example, the acrylic fiber was prepared by the following method:
(1) mixing far infrared component and polyethylene glycol, and grinding and dispersing under ultrasonic condition to obtain far infrared slurry with particle diameter of 0.1 μm and solid content of 5 wt%;
(2) mixing acrylonitrile, vinyl acetate and sodium methallyl sulfonate in a mass ratio of 13.26:1:0.38 with the far infrared slurry prepared in the step (1) in a mass ratio of 3:100, simultaneously adding a catalyst ammonium persulfate with a preparation concentration of 3.5%, an activator sodium bisulfite with a preparation concentration of 25%, an accelerator ferrous sulfate with a preparation concentration of 0.08%, an acid agent sulfuric acid with a preparation concentration of 7% and a dispersant desalted water with a pH value of 7.0 for polymerization, adding a catalyst, an activator, an accelerator and an acid agent in a mass ratio of 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 separation, filtration and drying to prepare a far infrared polymer; the vacuum degree of the filtration is-36 kPa, the back flushing pressure is 500kPa, the mass flow of flushing water is 9000kg/h, and the mass flow of spray water is 14500 kg/h; the drying is to dry the filtered far infrared wet polymer slurry to reduce the water content of the far infrared polymer to 1.2 wt%;
(3) and (3) dissolving the far infrared polymer prepared in the step (2) in dimethylacetamide to obtain a glue solution with the far infrared polymer content of 26.0 wt%, and performing wet spinning with the glue solution as a raw material and the setting pressure of 320kPa to obtain the far infrared acrylic fiber.
Comparative examples 1 to 3
Comparative examples 1 to 3 acrylic fibers were prepared on the basis of examples 1 to 3, respectively, without adding a far infrared component, and other implementation methods of comparative examples 1 to 3 were the same as those of examples 1 to 3.
Experimental example 1
In this experimental example, the intrinsic viscosity and the vinyl acetate content of the far infrared polymers prepared in the step (2) of examples 1 to 6 were measured, respectively, and the results are shown in table 1; then, the far infrared acrylic fibers prepared in examples 1 to 6 and comparative examples 1 to 3 were analyzed and tested, and the results are shown in table 2, and the details are as follows:
TABLE 1 far infrared polymer test data sheet
| Polymer viscosity (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 Total analysis results of far infrared fibers
From the above table, the far infrared acrylic fibers prepared in examples 1 to 6 have a high specific radiance within the range of the optimal infrared absorption wavelength of a human body, while the comparative examples 1 to 3 are acrylic fibers prepared by removing the far infrared component on the basis of examples 1 to 3, and compared with the elongation at break and the strength parameters, it can be seen that the far infrared component is introduced into the acrylic fibers in an in-situ polymerization manner, 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.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. The far infrared acrylic fiber is characterized in that the specific radiance of the far infrared acrylic fiber at the wavelength of 4-14 mu m is 0.82-0.89.
2. The far infrared acrylic fiber as claimed in claim 1, wherein the far infrared acrylic fiber has an elongation at break of 40 to 48% and a strength of 2.3 to 2.9 cN/dtex.
3. A method for preparing far infrared acrylic fiber as claimed in claim 1 or 2, wherein the method comprises:
(1) mixing the far infrared component and polyethylene glycol, and grinding and dispersing under ultrasonic condition to obtain far infrared slurry;
(2) adding a reaction monomer into the far infrared slurry prepared in the step (1), and simultaneously adding a catalyst, an accelerant, an activating agent, an acid agent and a dispersing agent to enable the monomer to generate in-situ polymerization reaction between the layers of the far infrared nano molecular structure to prepare far infrared polymer slurry, and then removing the monomer, filtering and drying the slurry to prepare a far infrared polymer;
(3) and (3) dissolving the far infrared polymer prepared in the step (2) in dimethylacetamide to obtain a glue solution, and performing wet solution spinning by taking the glue solution as a raw material to obtain 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 step (1) is 0.1 to 10 μm, and the solid content is 3.0 to 20.0 wt%; preferably, the particle size of the far infrared slurry is 0.2-1 μm, and the solid content is 5.0-15.0 wt%.
5. The method for preparing far infrared acrylic fiber according to claim 3, wherein 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.
6. The method for preparing far infrared acrylic fiber according to claim 3, wherein the mass ratio of far infrared components to reactive monomers contained in the far infrared slurry in the step (2) is 2-5: 100; the reaction monomer comprises acrylonitrile, vinyl acetate and sodium methyl propylene sulfonate in a mass ratio of 12-14: 1: 0.2-0.8; the far infrared component is selected from one or more of silicon oxide, aluminum oxide, sodium oxide, potassium oxide, calcium oxide, magnesium oxide, iron oxide and titanium oxide.
7. The method for preparing far infrared acrylic fiber according to claim 3, wherein the degree of vacuum of the filtration in the step (2) is-20 to-40 kPa, the back-blowing pressure is 200 to 600kPa, and the mass flow of the washing water is 8000 to 15000 kg/h; the mass flow of the spray water is 8000-15000 kg/h; preferably, the vacuum degree is-25 to-35 kPa, the back flushing pressure is 300 to 400kPa, the mass flow of flushing water is 10000 to 13000kg/h, and the mass flow of shower water is 10000 to 14000 kg/h.
8. The method for preparing far infrared acrylic fiber as claimed in claim 3, wherein the drying in the step (2) is drying the filtered far infrared wet polymer slurry to reduce the water content of the far infrared polymer to 0.5-4.5 wt%, preferably to 1.5-2.5 wt%.
9. The method for preparing far infrared acrylic fiber according to claim 3, characterized in that in the step (2), ammonium persulfate with the preparation concentration of 1.0-4.0% is selected as the catalyst, and the preferable preparation concentration of the ammonium persulfate is 2.5-3.5%; the activating agent is sodium bisulfite with a preparation concentration of 15.0-25.0%, and the preferable preparation concentration of the sodium bisulfite is 17-22%; the accelerator is ferrous sulfate with the preparation concentration of 0.06-0.14%, and the optimal preparation concentration of the ferrous sulfate is 0.08-0.12%; the acid agent is sulfuric acid with the preparation concentration of 7-15%, and the preferable preparation concentration of the sulfuric acid is 9-11%; the dispersing agent 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 activating agent, the promoter and the acid agent added into the reaction system is 28-30: 5-5.5: 0.7-0.9: 1.
10. The method for preparing far infrared acrylic fiber as claimed in claim 3, wherein in the step (3), the content of far infrared polymer in the glue solution is 24.0-26.0 wt%.
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