CN108642919B - Special high-temperature leveling agent for superfine fiber fabric - Google Patents

Special high-temperature leveling agent for superfine fiber fabric Download PDF

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CN108642919B
CN108642919B CN201810423548.5A CN201810423548A CN108642919B CN 108642919 B CN108642919 B CN 108642919B CN 201810423548 A CN201810423548 A CN 201810423548A CN 108642919 B CN108642919 B CN 108642919B
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polyglutamic acid
leveling agent
stirring
temperature
fiber fabric
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CN108642919A (en
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汪涛
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ANHUI LIDA CLOTHING Co.,Ltd.
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Anhui Lida Clothing Co ltd
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/52General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing synthetic macromolecular substances
    • D06P1/5264Macromolecular compounds obtained otherwise than by reactions involving only unsaturated carbon-to-carbon bonds
    • D06P1/5278Polyamides; Polyimides; Polylactames; Polyalkyleneimines
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G69/00Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
    • C08G69/02Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
    • C08G69/08Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
    • C08G69/10Alpha-amino-carboxylic acids
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    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/52General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing synthetic macromolecular substances
    • D06P1/5207Macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • D06P1/525Polymers of unsaturated carboxylic acids or functional derivatives thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/60General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing polyethers
    • D06P1/613Polyethers without nitrogen
    • D06P1/6131Addition products of hydroxyl groups-containing compounds with oxiranes
    • D06P1/6133Addition products of hydroxyl groups-containing compounds with oxiranes from araliphatic or aliphatic alcohols
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/64General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds without sulfate or sulfonate groups
    • D06P1/651Compounds without nitrogen
    • D06P1/65106Oxygen-containing compounds
    • D06P1/65118Compounds containing hydroxyl groups
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/64General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds without sulfate or sulfonate groups
    • D06P1/651Compounds without nitrogen
    • D06P1/65106Oxygen-containing compounds
    • D06P1/65125Compounds containing ester groups
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/64General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds without sulfate or sulfonate groups
    • D06P1/651Compounds without nitrogen
    • D06P1/65106Oxygen-containing compounds
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    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/673Inorganic compounds
    • D06P1/67383Inorganic compounds containing silicon

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  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention discloses a special high-temperature leveling agent for superfine fiber fabrics, which relates to the technical field of fabric dyeing, and the preparation method comprises the following steps: (1) pretreatment of polyglutamic acid, (2) chemical modification of polyglutamic acid, (3) preparation of auxiliary materials, and (4) preparation of a leveling agent. The molecular chain flexibility of the polyglutamic acid is enhanced through the low-temperature plasma treatment, so that the polyglutamic acid is used as a main component of a leveling agent and is firmly attached to superfine fibers, and the leveling effect is improved; and the carboxyl contained in the polyglutamic acid structure and the hydroxyl contained in the decyl glucoside structure are subjected to esterification reaction, so that the dye uptake and the leveling property are improved.

Description

Special high-temperature leveling agent for superfine fiber fabric
The technical field is as follows:
the invention relates to the technical field of fabric dyeing, in particular to a high-temperature leveling agent special for superfine fiber fabric.
Background art:
the superfine fiber has very fine fineness, greatly reduced rigidity, soft hand feeling, fine fiber, increased layered structure, increased specific surface area and capillary effect, fine reflected light inside the fiber, elegant silk luster, and excellent moisture absorption and dissipating performance. The clothing made of superfine fiber is comfortable, beautiful, warm-keeping, breathable, has better drapability and fullness, is obviously improved in the aspects of hydrophobicity and antifouling property, and can design different tissue structures by utilizing the characteristics of large specific surface area and softness so as to absorb more sunlight heat energy or dissipate body temperature more quickly, thereby playing the role of being warm in winter and cool in summer.
Meanwhile, due to the characteristics of high count and high density of the superfine fibers, the dyeing uniformity difficulty is higher than that of common fibers. The dye must well penetrate into the superfine fiber, and the traditional high-temperature leveling agent is not beneficial to helping the dye penetrate into the fiber due to the large molecular weight and the long carbon chain, and finally, the phenomenon of uneven dyeing often occurs when the superfine fiber is dyed.
The invention content is as follows:
the invention aims to solve the technical problem of providing the special high-temperature leveling agent for the superfine fiber fabric, which can obviously reduce color difference, improve the utilization rate of dye and improve color fastness.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
a high-temperature leveling agent special for superfine fiber fabrics is prepared by the following steps:
(1) pretreatment of polyglutamic acid: putting polyglutamic acid into a vacuum chamber of a plasma reactor, vacuumizing to 1Pa, introducing nitrogen until the pressure of the vacuum chamber reaches 10Pa, controlling the temperature at 45-55 ℃, controlling the discharge power at 450W, stopping discharging after continuously discharging for 3-8 min, uniformly stirring, continuously discharging for 3-8 min again after 10min, and stopping discharging;
(2) chemical modification of polyglutamic acid: adding water into pretreated polyglutamic acid and decyl glucoside, stirring, dissolving completely, then dropwise adding 98% concentrated sulfuric acid to adjust the pH value to 4, heating to 60-70 ℃, keeping the temperature, stirring, reacting, concentrating under reduced pressure to obtain paste, naturally cooling the paste to room temperature, then feeding the paste into a freeze dryer, drying the obtained solid, and micronizing to obtain modified polyglutamic acid;
(3) preparing auxiliary materials: heating cetyl alcohol to molten state, stirring under heat preservation, adding allyl glycidyl ether and isooctyl palmitate, and mixing to obtain adjuvants;
(4) preparation of leveling agent: and (3) uniformly mixing the prepared modified polyglutamic acid and auxiliary materials, heating to 110-120 ℃ at a heating rate of 5 ℃/min, stirring for 5-10 min at a heat preservation temperature, cooling to-10-0 ℃ at a cooling rate of 5 ℃/min, stirring for 5-10 min at a heat preservation temperature, and naturally returning to room temperature to obtain the leveling agent.
The polyglutamic acid is water treatment grade polyglutamic acid.
The mass ratio of the polyglutamic acid to the decyl glucoside to the cetyl alcohol to the allyl glycidyl ether to the isooctyl palmitate is 50: 10-20: 1-10.
The auxiliary material also comprises nanometer rubber powder, and the mass ratio of the nanometer rubber powder to the polyglutamic acid is 1-10: 50.
The nanometer rubber powder is prepared from gas-phase silicon dioxide, PEG-60 hydrogenated castor oil and hydrolyzed polymaleic anhydride, and the preparation method comprises the following steps: fully mixing the gas-phase silicon dioxide, the PEG-60 hydrogenated castor oil and the hydrolyzed polymaleic anhydride, then granulating by a dry method to prepare particles of 60-80 meshes, and finally preparing the particles into nano powder by a nano grinder to obtain the nano rubber powder.
The mass ratio of the fumed silica to the PEG-60 hydrogenated castor oil to the hydrolyzed polymaleic anhydride is 3:2: 0.5.
The invention has the beneficial effects that:
(1) the molecular chain flexibility of the polyglutamic acid is enhanced through the low-temperature plasma treatment, so that the polyglutamic acid is used as a main component of a leveling agent and is firmly attached to superfine fibers, and the leveling effect is improved;
(2) the carboxyl contained in the polyglutamic acid structure and the hydroxyl contained in the decyl glucoside structure are subjected to esterification reaction, so that the hydroxyl is introduced into the polyglutamic acid structure, the prepared modified polyglutamic acid structure simultaneously contains three active groups, namely carboxyl, amino and hydroxyl, and the dye molecules are favorably and stably combined on superfine fibers through the existence of the active groups;
(3) according to the invention, the leveling property of the prepared leveling agent is enhanced through the matching use of auxiliary materials, the color difference is reduced, and the uniform dyeing of the superfine fiber fabric is realized; particularly, the prepared leveling agent has super-strong permeability by adding the nanometer rubber powder, so that the leveling agent enters the superfine fiber under the permeation action, and the color fastness of the superfine fiber fabric is improved;
(4) according to the invention, the temperature sensitivity of the leveling agent is reduced through the procedure heating and cooling treatment of the final stage of the leveling agent preparation, so that the leveling agent can play an excellent leveling effect no matter in a low-temperature environment or a high-temperature environment.
The specific implementation mode is as follows:
in order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Example 1
(1) Pretreatment of polyglutamic acid: putting 50g of water treatment-grade polyglutamic acid into a vacuum chamber of a plasma reactor, vacuumizing to 1Pa, introducing nitrogen until the pressure of the vacuum chamber reaches 10Pa, controlling the temperature at 55 ℃ and the discharge power at 450W, stopping discharging after continuously discharging for 5min, uniformly stirring, continuously discharging for 5min again after 10min, and stopping discharging;
(2) chemical modification of polyglutamic acid: adding water into pretreated polyglutamic acid and 10g decyl glucoside, stirring, dissolving completely, adding 98% concentrated sulfuric acid dropwise to adjust pH value to 4, heating to 70 ℃, keeping the temperature, stirring, reacting, concentrating under reduced pressure to obtain paste, naturally cooling to room temperature, feeding into a freeze dryer, drying to obtain solid, and micronizing to obtain modified polyglutamic acid;
(3) preparing auxiliary materials: heating 3g of cetyl alcohol to a molten state, preserving heat, stirring, adding 2g of allyl glycidyl ether and 2g of isooctyl palmitate, and uniformly mixing to obtain an auxiliary material;
(4) preparation of leveling agent: and (3) uniformly mixing the prepared modified polyglutamic acid and auxiliary materials, heating to 110 ℃ at the heating rate of 5 ℃/min, keeping the temperature, stirring for 10min, cooling to-10 ℃ at the cooling rate of 5 ℃/min, keeping the temperature, stirring for 10min, and naturally returning to the room temperature to obtain the leveling agent.
Example 2
(1) Pretreatment of polyglutamic acid: putting 50g of water treatment-grade polyglutamic acid into a vacuum chamber of a plasma reactor, vacuumizing to 1Pa, introducing nitrogen until the pressure of the vacuum chamber reaches 10Pa, controlling the temperature at 55 ℃ and the discharge power at 450W, stopping discharging after continuously discharging for 5min, uniformly stirring, continuously discharging for 5min again after 10min, and stopping discharging;
(2) chemical modification of polyglutamic acid: adding water into pretreated polyglutamic acid and 15g decyl glucoside, stirring, dissolving completely, adding 98% concentrated sulfuric acid dropwise to adjust pH value to 4, heating to 70 ℃, keeping the temperature, stirring, reacting, concentrating under reduced pressure to obtain paste, naturally cooling to room temperature, feeding into a freeze dryer, drying to obtain solid, and micronizing to obtain modified polyglutamic acid;
(3) preparing auxiliary materials: heating 3g of cetyl alcohol to a molten state, preserving heat, stirring, adding 3g of allyl glycidyl ether and 2g of isooctyl palmitate, and uniformly mixing to obtain an auxiliary material;
(4) preparation of leveling agent: and (3) uniformly mixing the prepared modified polyglutamic acid and auxiliary materials, heating to 110 ℃ at the heating rate of 5 ℃/min, keeping the temperature, stirring for 10min, cooling to-10 ℃ at the cooling rate of 5 ℃/min, keeping the temperature, stirring for 10min, and naturally returning to the room temperature to obtain the leveling agent.
Example 3
(1) Pretreatment of polyglutamic acid: putting 50g of water treatment-grade polyglutamic acid into a vacuum chamber of a plasma reactor, vacuumizing to 1Pa, introducing nitrogen until the pressure of the vacuum chamber reaches 10Pa, controlling the temperature at 55 ℃ and the discharge power at 450W, stopping discharging after continuously discharging for 5min, uniformly stirring, continuously discharging for 5min again after 10min, and stopping discharging;
(2) chemical modification of polyglutamic acid: adding water into pretreated polyglutamic acid and 15g decyl glucoside, stirring, dissolving completely, adding 98% concentrated sulfuric acid dropwise to adjust pH value to 4, heating to 70 ℃, keeping the temperature, stirring, reacting, concentrating under reduced pressure to obtain paste, naturally cooling to room temperature, feeding into a freeze dryer, drying to obtain solid, and micronizing to obtain modified polyglutamic acid;
(3) preparing auxiliary materials: heating 3g of cetyl alcohol to a molten state, preserving heat, stirring, adding 3g of allyl glycidyl ether, 2.5g of nano rubber powder and 2g of isooctyl palmitate, and uniformly mixing to obtain an auxiliary material;
(4) preparation of leveling agent: and (3) uniformly mixing the prepared modified polyglutamic acid and auxiliary materials, heating to 110 ℃ at the heating rate of 5 ℃/min, keeping the temperature, stirring for 10min, cooling to-10 ℃ at the cooling rate of 5 ℃/min, keeping the temperature, stirring for 10min, and naturally returning to the room temperature to obtain the leveling agent.
Preparing the nanometer rubber powder: fully mixing 3g of fumed silica, 2g of PEG-60 hydrogenated castor oil and 0.5g of hydrolyzed polymaleic anhydride, granulating by a dry method to prepare particles of 60-80 meshes, and finally preparing the particles into nano powder by a nano grinder to obtain the nano rubber powder.
Comparative example 1
(1) Pretreatment of polyglutamic acid: putting 50g of water treatment-grade polyglutamic acid into a vacuum chamber of a plasma reactor, vacuumizing to 1Pa, introducing nitrogen until the pressure of the vacuum chamber reaches 10Pa, controlling the temperature at 55 ℃ and the discharge power at 450W, stopping discharging after continuously discharging for 5min, uniformly stirring, continuously discharging for 5min again after 10min, and stopping discharging;
(2) chemical modification of polyglutamic acid: adding water into pretreated polyglutamic acid and 15g decyl glucoside, stirring, dissolving completely, adding 98% concentrated sulfuric acid dropwise to adjust pH value to 4, heating to 70 ℃, keeping the temperature, stirring, reacting, concentrating under reduced pressure to obtain paste, naturally cooling to room temperature, feeding into a freeze dryer, drying to obtain solid, and micronizing to obtain modified polyglutamic acid;
(3) preparing auxiliary materials: heating 3g of cetyl alcohol to a molten state, preserving heat, stirring, adding 3g of allyl glycidyl ether and 2g of isooctyl palmitate, and uniformly mixing to obtain an auxiliary material;
(4) preparation of leveling agent: and (3) uniformly mixing the prepared modified polyglutamic acid and auxiliary materials to obtain the leveling agent.
Comparative example 2
(1) Pretreatment of polyglutamic acid: putting 50g of water treatment-grade polyglutamic acid into a vacuum chamber of a plasma reactor, vacuumizing to 1Pa, introducing nitrogen until the pressure of the vacuum chamber reaches 10Pa, controlling the temperature at 55 ℃ and the discharge power at 450W, stopping discharging after continuously discharging for 5min, uniformly stirring, continuously discharging for 5min again after 10min, and stopping discharging;
(2) chemical modification of polyglutamic acid: adding water into pretreated polyglutamic acid and 15g decyl glucoside, stirring, dissolving completely, adding 98% concentrated sulfuric acid dropwise to adjust pH value to 4, heating to 70 ℃, keeping the temperature, stirring, reacting, concentrating under reduced pressure to obtain paste, naturally cooling to room temperature, feeding into a freeze dryer, drying to obtain solid, and micronizing to obtain modified polyglutamic acid;
(3) preparing auxiliary materials: heating 3g of cetyl alcohol to a molten state, keeping the temperature, stirring, adding 3g of allyl glycidyl ether, and uniformly mixing to obtain an auxiliary material;
(4) preparation of leveling agent: and (3) uniformly mixing the prepared modified polyglutamic acid and auxiliary materials, heating to 110 ℃ at the heating rate of 5 ℃/min, keeping the temperature, stirring for 10min, cooling to-10 ℃ at the cooling rate of 5 ℃/min, keeping the temperature, stirring for 10min, and naturally returning to the room temperature to obtain the leveling agent.
Comparative example 3
(1) Pretreatment of polyglutamic acid: putting 50g of water treatment-grade polyglutamic acid into a vacuum chamber of a plasma reactor, vacuumizing to 1Pa, introducing nitrogen until the pressure of the vacuum chamber reaches 10Pa, controlling the temperature at 55 ℃ and the discharge power at 450W, stopping discharging after continuously discharging for 5min, uniformly stirring, continuously discharging for 5min again after 10min, and stopping discharging;
(2) chemical modification of polyglutamic acid: adding water into pretreated polyglutamic acid and 15g decyl glucoside, stirring, dissolving completely, adding 98% concentrated sulfuric acid dropwise to adjust pH value to 4, heating to 70 ℃, keeping the temperature, stirring, reacting, concentrating under reduced pressure to obtain paste, naturally cooling to room temperature, feeding into a freeze dryer, drying to obtain solid, and micronizing to obtain modified polyglutamic acid;
(3) preparing auxiliary materials: heating 3g of cetyl alcohol to a molten state, keeping the temperature, stirring, adding 2g of isooctyl palmitate, and uniformly mixing to obtain an auxiliary material;
(4) preparation of leveling agent: and (3) uniformly mixing the prepared modified polyglutamic acid and auxiliary materials, heating to 110 ℃ at the heating rate of 5 ℃/min, keeping the temperature, stirring for 10min, cooling to-10 ℃ at the cooling rate of 5 ℃/min, keeping the temperature, stirring for 10min, and naturally returning to the room temperature to obtain the leveling agent.
Comparative example 4
(1) Pretreatment of polyglutamic acid: putting 50g of water treatment-grade polyglutamic acid into a vacuum chamber of a plasma reactor, vacuumizing to 1Pa, introducing nitrogen until the pressure of the vacuum chamber reaches 10Pa, controlling the temperature at 55 ℃ and the discharge power at 450W, stopping discharging after continuously discharging for 5min, uniformly stirring, continuously discharging for 5min again after 10min, and stopping discharging;
(2) chemical modification of polyglutamic acid: adding water into pretreated polyglutamic acid and 15g decyl glucoside, stirring, dissolving completely, adding 98% concentrated sulfuric acid dropwise to adjust pH value to 4, heating to 70 ℃, keeping the temperature, stirring, reacting, concentrating under reduced pressure to obtain paste, naturally cooling to room temperature, feeding into a freeze dryer, drying to obtain solid, and micronizing to obtain modified polyglutamic acid;
(3) preparation of leveling agent: heating the prepared modified polyglutamic acid to 110 ℃ at the heating rate of 5 ℃/min, stirring for 10min while keeping the temperature, cooling to-10 ℃ at the cooling rate of 5 ℃/min, stirring for 10min while keeping the temperature, and naturally recovering to room temperature to obtain the leveling agent.
Comparative example 5
(1) Chemical modification of polyglutamic acid: adding water into 50g of water treatment-grade polyglutamic acid and 15g of decyl glucoside, stirring, dissolving completely, then dropwise adding 98% concentrated sulfuric acid to adjust the pH value to 4, heating to 70 ℃, keeping the temperature, stirring, reacting, concentrating under reduced pressure to obtain paste, naturally cooling the paste to room temperature, then sending the paste into a freeze dryer, drying the obtained solid, and preparing the dried solid into micropowder by using an ultrafine pulverizer to obtain modified polyglutamic acid;
(2) preparing auxiliary materials: heating 3g of cetyl alcohol to a molten state, preserving heat, stirring, adding 3g of allyl glycidyl ether and 2g of isooctyl palmitate, and uniformly mixing to obtain an auxiliary material;
(3) preparation of leveling agent: and (3) uniformly mixing the prepared modified polyglutamic acid and auxiliary materials, heating to 110 ℃ at the heating rate of 5 ℃/min, keeping the temperature, stirring for 10min, cooling to-10 ℃ at the cooling rate of 5 ℃/min, keeping the temperature, stirring for 10min, and naturally returning to the room temperature to obtain the leveling agent.
Comparative example 6
(1) Pretreatment of polyglutamic acid: putting 50g of water treatment-grade polyglutamic acid into a vacuum chamber of a plasma reactor, vacuumizing to 1Pa, introducing nitrogen until the pressure of the vacuum chamber reaches 10Pa, controlling the temperature at 55 ℃ and the discharge power at 450W, stopping discharging after continuously discharging for 5min, uniformly stirring, continuously discharging for 5min again after 10min, and stopping discharging;
(2) preparing auxiliary materials: heating 3g of cetyl alcohol to a molten state, preserving heat, stirring, adding 3g of allyl glycidyl ether and 2g of isooctyl palmitate, and uniformly mixing to obtain an auxiliary material;
(3) preparation of leveling agent: uniformly mixing the pretreated polyglutamic acid and the prepared auxiliary materials, heating to 110 ℃ at the heating rate of 5 ℃/min, stirring for 10min at the heat preservation temperature, cooling to-10 ℃ at the cooling rate of 5 ℃/min, stirring for 10min at the heat preservation temperature, and naturally returning to the room temperature to obtain the leveling agent.
Example 4
Based on example 2, there were provided comparative example 1 in which temperature programming and temperature reduction treatment were not performed at the time of preparing the leveling agent, comparative example 2 in which isooctyl palmitate was not added at the time of preparing the auxiliary material, comparative example 3 in which allyl glycidyl ether was not added at the time of preparing the auxiliary material, comparative example 4 in which the auxiliary material was not added at the time of preparing the leveling agent, comparative example 5 in which pretreatment was not performed, and comparative example 6 in which chemical modification was not performed.
Examples 1 to 3 and comparative examples 1 to 6 were used to prepare leveling agents, and the same amount of the leveling agents thus prepared was used for dyeing the same amount of ultrafine fiber fabrics in the same lot by the same dyeing process, while a blank example without using the leveling agent was set, and the dyeing effect was measured, as shown in table 1.
The larger the K/S value is, the more the combination amount of the dye and the superfine fiber is, and the higher the dye uptake is; the smaller the DEcmc value is, the better the leveling property is; the higher the washing fastness grade value is, the better the color fastness is represented.
TABLE 1 levelling Properties of levelling agents prepared according to the invention
Figure BDA0001651378980000071
Figure BDA0001651378980000081
The dyeing process comprises the following steps: putting 250g of superfine fiber fabric into a roller dyeing machine, adding 2000g of water, completely wetting the fabric, adding 5g of leveling agent, rotating for 15min, adding 10g of dye, continuously rotating for 60min, washing with water, and drying to finish dyeing.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (6)

1. The special high-temperature leveling agent for the superfine fiber fabric is characterized by comprising the following steps of:
(1) pretreatment of polyglutamic acid: putting polyglutamic acid into a vacuum chamber of a plasma reactor, vacuumizing to 1Pa, introducing nitrogen until the pressure of the vacuum chamber reaches 10Pa, controlling the temperature at 45-55 ℃, controlling the discharge power at 450W, stopping discharging after continuously discharging for 3-8 min, uniformly stirring, continuously discharging for 3-8 min again after 10min, and stopping discharging;
(2) chemical modification of polyglutamic acid: adding water into pretreated polyglutamic acid and decyl glucoside, stirring, dissolving completely, then dropwise adding 98% concentrated sulfuric acid to adjust the pH value to 4, heating to 60-70 ℃, keeping the temperature, stirring, reacting, concentrating under reduced pressure to obtain paste, naturally cooling the paste to room temperature, then feeding the paste into a freeze dryer, drying the obtained solid, and micronizing to obtain modified polyglutamic acid;
(3) preparing auxiliary materials: heating cetyl alcohol to molten state, stirring under heat preservation, adding allyl glycidyl ether and isooctyl palmitate, and mixing to obtain adjuvants;
(4) preparation of leveling agent: and (3) uniformly mixing the prepared modified polyglutamic acid and auxiliary materials, heating to 110-120 ℃ at a heating rate of 5 ℃/min, stirring for 5-10 min at a heat preservation temperature, cooling to-10-0 ℃ at a cooling rate of 5 ℃/min, stirring for 5-10 min at a heat preservation temperature, and naturally returning to room temperature to obtain the leveling agent.
2. The high temperature leveling agent special for the ultrafine fiber fabric according to claim 1, wherein: the polyglutamic acid is water treatment grade polyglutamic acid.
3. The high temperature leveling agent special for the ultrafine fiber fabric according to claim 1, wherein: the mass ratio of the polyglutamic acid to the decyl glucoside to the cetyl alcohol to the allyl glycidyl ether to the isooctyl palmitate is 50: 10-20: 1-10.
4. The high temperature leveling agent special for the ultrafine fiber fabric according to claim 1, wherein: the auxiliary material also comprises nanometer rubber powder, and the mass ratio of the nanometer rubber powder to the polyglutamic acid is 1-10: 50.
5. The high temperature leveling agent special for the ultrafine fiber fabric according to claim 4, wherein: the nanometer rubber powder is prepared from gas-phase silicon dioxide, PEG-60 hydrogenated castor oil and hydrolyzed polymaleic anhydride, and the preparation method comprises the following steps: fully mixing the gas-phase silicon dioxide, the PEG-60 hydrogenated castor oil and the hydrolyzed polymaleic anhydride, then granulating by a dry method to prepare particles of 60-80 meshes, and finally preparing the particles into nano powder by a nano grinder to obtain the nano rubber powder.
6. The high temperature leveling agent special for the ultrafine fiber fabric according to claim 5, wherein: the mass ratio of the fumed silica to the PEG-60 hydrogenated castor oil to the hydrolyzed polymaleic anhydride is 3:2: 0.5.
CN201810423548.5A 2018-05-06 2018-05-06 Special high-temperature leveling agent for superfine fiber fabric Active CN108642919B (en)

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CN111139665B (en) * 2019-12-31 2022-11-11 郎溪远华纺织有限公司 Dyeing process of high-precision flat shading cloth
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