CN111676536A - Preparation method of temperature-adjusting microcapsule and graphene compounded viscose fiber - Google Patents

Preparation method of temperature-adjusting microcapsule and graphene compounded viscose fiber Download PDF

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Publication number
CN111676536A
CN111676536A CN202010506609.1A CN202010506609A CN111676536A CN 111676536 A CN111676536 A CN 111676536A CN 202010506609 A CN202010506609 A CN 202010506609A CN 111676536 A CN111676536 A CN 111676536A
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temperature
graphene
microcapsule
viscose fiber
preparation
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CN202010506609.1A
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Inventor
王进美
王志强
畅娇
刘红媛
华炳宇
王新
刘荣欣
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Xianyang Textile Group Co ltd
Xian Polytechnic University
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Xianyang Textile Group Co ltd
Xian Polytechnic University
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Priority to CN202010506609.1A priority Critical patent/CN111676536A/en
Publication of CN111676536A publication Critical patent/CN111676536A/en
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D01F2/06Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
    • D01F2/08Composition of the spinning solution or the bath

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Artificial Filaments (AREA)

Abstract

The invention discloses a preparation method of a temperature-adjusting microcapsule and graphene compounded viscose fiber, which specifically comprises the following steps: adding 8-10 parts of temperature-adjusting microcapsules and 1-3 parts of graphene powder into 1000 parts of viscose spinning coagulating bath containing 8-9% of cellulose according to the weight ratio, uniformly stirring, then grinding, dissolving, ripening, defoaming, ripening, filtering twice, degassing in a degassing tank, spinning by a spinning machine, and processing into viscose fiber compounded by the temperature-adjusting microcapsules and the graphene with certain length, titer and curling according to the requirements. According to the preparation method of the viscose fiber compounded by the temperature-regulating microcapsule and the graphene, the composite viscose fiber prepared by compounding the phase-change temperature regulation and the graphene has good thermal comfort and good antistatic, antibacterial and uvioresistant performances.

Description

Preparation method of temperature-adjusting microcapsule and graphene compounded viscose fiber
Technical Field
The invention belongs to the technical field of textiles, and relates to a preparation method of a temperature-regulating microcapsule and graphene compounded viscose fiber.
Background
In recent years, with the improvement of living standard quality, people pursue clothing products more and pay more attention to comfort and functionality. At present, the processing technology of the phase change thermoregulation fiber and the graphene fiber with single function is gradually mature, and has certain large-scale application. However, no relevant report is found on fibers combining phase change temperature adjustment and antibacterial, antistatic and ultraviolet resistant functions of graphene. By utilizing the temperature adjusting effect of the phase-change material and the characteristics of ultrahigh specific surface area, good flexibility, excellent conductivity and the like of the graphene, the textile composite material with the good temperature adjusting effect and the composite functions of antibiosis, static resistance and ultraviolet resistance is developed, and the thermal comfort and safety of people can be obviously improved.
Disclosure of Invention
The invention aims to provide a preparation method of a viscose fiber compounded by temperature-regulating microcapsules and graphene, and the composite viscose fiber prepared by compounding phase-change temperature regulation and graphene has good thermal comfort and good antistatic, antibacterial and uvioresistant properties.
The invention adopts the technical scheme that a preparation method of a temperature-regulating microcapsule and graphene compounded viscose fiber specifically comprises the following steps: adding 8-10 parts of temperature-adjusting microcapsules and 1-3 parts of graphene powder into 1000 parts of viscose spinning coagulating bath containing 8-9% of cellulose according to the weight ratio, uniformly stirring, then grinding, dissolving, ripening, defoaming, ripening, filtering twice, degassing in a degassing tank, spinning by a spinning machine, and processing into viscose fiber compounded by the temperature-adjusting microcapsules and the graphene with certain length, titer and curling according to the requirements.
The present invention is also characterized in that,
the temperature-regulating microcapsule comprises a core material, wherein the core material is coated with a first layer of shell material, the first layer of shell material is coated with a second layer of shell material, and the temperature-regulating microcapsule specifically comprises the following components in percentage by mass: the core material is waste swill recovered animal and plant modified grease: 50-60%, the first layer of shell material is gelatin: 10-20% of the second layer of shell material, and 20-35% of the aqueous polyurethane solution.
The preparation method of the temperature-regulating microcapsule comprises the following steps:
step 1, preparing waste swill and recovering animal and plant modified grease;
step 2, coating the animal and plant modified grease recovered from the waste swill prepared in the step 1 in gelatin by adopting a coating method to obtain gelatin-coated modified grease microcapsule particles;
and 3, coating the gelatin-coated modified grease microcapsule particles obtained in the step 2 in an aqueous polyurethane solution by adopting a coating method to form temperature-regulating microcapsule particles.
The step 1 specifically comprises the following steps: the preparation method of the animal and plant modified grease recovered from waste swill comprises the following steps: recovering the waste swill from the animal and plant modified grease, introducing hydrogen into a closed reaction kettle, and carrying out hydrogenation treatment for 6-8 hours at the temperature of 120-130 ℃ and the pressure of 1.8-2.0MPa to obtain the animal and plant modified grease recovered from the waste swill.
The step 2 specifically comprises the following steps: adding the animal and plant modified grease recovered from the waste swill prepared in the step 1 into 10-20% gelatin solution, shearing at high speed for 20-30 minutes under the condition of 16000-.
The weight ratio of the animal and plant modified grease recovered from waste swill to 10-20% gelatin solution is: 5-6: 10.
the step 3 specifically comprises the following steps:
adding the gelatin-coated modified grease microcapsule particles into 10-20% aqueous polyurethane solution, shearing at high speed for 15-20 minutes under the conditions of 16000 and 18000 revolutions per minute, and carrying out vacuum concentration and drying for 6-8 hours under the stirring state to form the temperature-regulating microcapsule particles.
The weight ratio of the gelatin coated modified grease microcapsule particles to the 10-20% aqueous polyurethane solution is as follows: 6-8:10.
The invention has the beneficial effects that the invention adopts a complex phase double-layer coating method to prepare the phase-change material microcapsule, then mixes the prepared temperature-adjusting microcapsule, the graphene powder and the adhesive according to a certain proportion, adds the mixture into the coagulating bath of the viscose fiber by a two-bath method, and then passes through a series of conventional silk-making processes,DSC test results show that the temperature adjusting range of the phase change temperature adjusting graphene fiber is 19.56-31.53 ℃, the peak value is 24.32-27.69 ℃, the solidification temperature range is 18.46-23.46 ℃, the temperature is just in the comfortable temperature range of human bodies, in addition, the melting heat of the phase change temperature adjusting graphene fiber is 41.56-56.29J/g, the solidification heat is 43.15-49.81J/g, the viscose fiber has a large energy storage effect, and the fiber mass specific resistance is 6.33-9.84 × 107Omega, the enthalpy value of phase change is 35.26-44.39J/g, the bacteriostatic rates of staphylococcus aureus, escherichia coli and candida albicans are all more than 95%, the ultraviolet shielding rate UPF of the prepared plain weave fabric is improved by 50-90% compared with the ordinary viscose fiber without the phase change microcapsule and the graphene, the fabric has good antistatic, antibacterial and uvioresistant performances, after 50 times of washing, the performance reduction is less than 5%, the fabric can be widely applied to processing various temperature-adjusting graphene composite functional textiles so as to meet the requirements of textile clothing products for household, outdoor, occupation and the like, and has important social and economic significance.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The invention relates to a preparation method of a temperature-regulating microcapsule and graphene compounded viscose fiber, which specifically comprises the following steps:
adding 8-10 parts of temperature-adjusting microcapsules and 1-3 parts of graphene powder into 1000 parts of viscose spinning coagulating bath containing 8-9% of cellulose according to the weight ratio, uniformly stirring, then grinding, dissolving, ripening, defoaming, ripening, filtering twice, degassing in a degassing tank, spinning by a spinning machine, and processing into viscose fiber compounded by the temperature-adjusting microcapsules and the graphene with certain length, titer and curling according to the requirements.
The temperature-regulating microcapsule comprises a core material, wherein the core material is coated with a first layer of shell material, the first layer of shell material is coated with a second layer of shell material, and the temperature-regulating microcapsule specifically comprises the following components in percentage by mass: the core material is waste swill recovered animal and plant modified grease: 50-60%, the first layer of shell material is gelatin: 10-20% of the second layer of shell material, and 20-35% of the aqueous polyurethane solution.
The preparation method of the temperature-regulating microcapsule comprises the following steps:
step 1, recovering grease from waste swill, introducing hydrogen into a closed reaction kettle, and carrying out hydrogenation treatment for 6 hours at the temperature of 120-;
step 2, adding the waste swill recovered animal and plant modified grease prepared in the step 1 into 10-20% gelatin solution, shearing at high speed for 20-30 minutes under the condition of 16000-: 5-6: 10;
step 3, adding the gelatin-coated modified oil microcapsule particles into 10-20% aqueous polyurethane solution, shearing at high speed for 15-20 minutes under the condition of 16000-: 6-8:10.
Example 1
1. The temperature-regulating microcapsule comprises the following components in percentage by mass: the core material is waste swill recovered animal and plant modified grease: 50%, the first layer shell material is gelatin: 10 percent, and the second layer shell material is 20 percent of aqueous polyurethane solution;
wherein, the animal and plant modified grease recovered from waste swill is the waste swill recovered grease, hydrogen is introduced into a closed reaction kettle, and the mixture is hydrogenated for 6 hours at the temperature of 130 ℃ under the pressure of 1.8 MPa;
the first shell material coating method comprises the following steps: adding 100 parts by weight of 10% gelatin solution into 50 parts by weight of animal and vegetable modified oil recovered from waste swill, shearing at high speed for 20 minutes under the condition of 16000 r/min, and carrying out vacuum concentration and drying for 5 hours under the stirring state to form gelatin-coated modified oil microcapsule particles.
The second layer of shell material coating method comprises the following steps: 60 parts of gelatin-coated modified oil microcapsule particles are added into 100 parts (by weight) of 10% aqueous polyurethane solution, and are sheared at high speed for 15 minutes under the condition of 16000 r/min, and are dried for 6 hours under vacuum concentration under the stirring state. Forming temperature-regulating microcapsule particles.
2. The preparation method of the viscose fiber compounded by the temperature-adjusting microcapsule and the graphene comprises the following steps: mixing 8 parts (by weight) of temperature-adjusting microcapsule, graphene powder: 1 part of the temperature-regulating microcapsule graphene composite functional viscose fiber is added into 1000 parts of viscose spinning coagulating bath containing 9 percent of cellulose, is stirred uniformly by strong force, is subjected to subsequent grinding, dissolution, ripening, defoaming, ripening, secondary filtering, degassing in a degassing tank and spinning by a spinning machine according to a conventional process, and is processed into the temperature-regulating microcapsule graphene composite functional viscose fiber with the length of 38mm, the fineness of 1.5D and the crimp of 5 pieces/cm according to requirements.
DSC test results of the temperature-regulating microcapsule graphene composite functional viscose fiber prepared by testing show that the temperature regulating range of the phase-change temperature-regulating graphene fiber is 19.56-30.68 ℃, the peak value is 24.32 ℃, the solidification temperature range is 18.46-22.78 ℃, the melting heat of the phase-change temperature-regulating graphene fiber is 41.56J/g, the solidification heat is 43.15J/g, and the mass specific resistance of the fiber is 6.33 × 107Omega, the enthalpy of phase transition is 35.26J/g, and the bacteriostatic rates of staphylococcus aureus, escherichia coli and candida albicans are respectively as follows: 99.1 percent, 99.3 percent and 96.4 percent, and the ultraviolet shielding rate UPF of the plain weave fabric is improved by 50 percent compared with the common viscose fiber without the phase change microcapsule and the graphene. Has good antistatic, antibacterial and uvioresistant performances. After 50 times of washing, the performance reduction of each type is less than 5 percent.
Example 2
1. The temperature-regulating microcapsule comprises the following components in percentage by mass: 60%, the first layer shell material is gelatin: 15 percent, and the second layer shell material is 35 percent of aqueous polyurethane solution.
Wherein, the animal and plant modified grease recovered from waste swill is the waste swill recovered grease, and hydrogen is introduced into a closed reaction kettle and is subjected to hydrogenation treatment for 8 hours at 120 ℃ under 2.0 MPa.
The first shell material coating method comprises the following steps: adding 100 parts by weight of 15% gelatin solution into 60 parts by weight of animal and plant modified oil recovered from waste swill, and shearing at high speed for 30 minutes under the condition of 18000 r/min. And (3) concentrating and drying for 6 hours under the stirring state in vacuum to form the gelatin-coated modified oil microcapsule particles.
The second layer of shell material coating method comprises the following steps: adding 75 parts by weight of gelatin-coated modified oil microcapsule particles into 100 parts by weight of 20% aqueous polyurethane solution, shearing at a high speed of 18000 r/min for 30 min, and carrying out vacuum concentration and drying for 8 h under a stirring state to form temperature-regulating microcapsule particles.
2. The preparation method of the viscose fiber compounded by the temperature-adjusting microcapsule and the graphene comprises the following steps: 10 parts (by weight) of temperature-adjusting microcapsule, graphene powder: and 3 parts of the temperature-regulating microcapsule graphene composite functional viscose fiber with the length of 68mm, the fineness of 3D and the crimp of 4 pieces/cm is processed according to requirements by adding 1000 parts of the temperature-regulating microcapsule graphene composite functional viscose fiber into 8 percent viscose spinning coagulating bath containing cellulose, strongly stirring the mixture uniformly, finishing subsequent grinding, dissolving, ripening, defoaming, ripening, secondary filtering, degassing in a degassing tank and spinning in a spinning machine according to a conventional process.
The method has the beneficial effects that the phase change material microcapsules are prepared by adopting a complex phase double-layer coating method, then the prepared phase change microcapsules, the graphene material and the adhesive are mixed according to a certain proportion, the mixture is added into a coagulating bath of viscose fibers prepared by a two-bath method, and then a series of conventional silk making processes are carried out to prepare the temperature-regulating microcapsule graphene composite functional viscose fibers7Omega, the enthalpy of phase transition is 44.39J/g, and the bacteriostatic rates of staphylococcus aureus, escherichia coli and candida albicans are respectively as follows: 99.9 percent, 99.9 percent and 99.2 percent, and the ultraviolet shielding rate UPF of the plain weave fabric is improved by 90 percent compared with the common viscose fiber without the phase-change microcapsule and the graphene. Has good antistatic, antibacterial and uvioresistant performances. After 50 times of washing, the performance reduction of each type is less than 5 percent.
Example 3
1. The temperature-regulating microcapsule comprises the following components in percentage by mass: 55%, the first layer shell material is gelatin: 15 percent, and the second layer shell material is 30 percent of aqueous polyurethane solution.
Wherein, the animal and plant modified grease recovered from waste swill is the waste swill recovered grease, and hydrogen is introduced into a closed reaction kettle and is subjected to hydrogenation treatment for 7 hours at the temperature of 125 ℃ and the pressure of 1.9 MPa.
The first shell material coating method comprises the following steps: adding 100 parts by weight of 15% gelatin solution into 55 parts by weight of animal and vegetable modified oil recovered from waste swill, shearing at a high speed for 25 minutes under the condition of 17000 r/min, and carrying out vacuum concentration and drying for 5.5 hours under the stirring state to form gelatin-coated modified oil microcapsule particles.
The second layer of shell material coating method comprises the following steps: 70 parts of gelatin-coated modified oil microcapsule particles are added into 100 parts (by weight) of 30% aqueous polyurethane solution, and high-speed shearing is carried out for 18 minutes under the condition of 16000 r/min. And concentrating and drying for 7 hours in vacuum under the stirring state to form the temperature-regulating microcapsule particles.
2. The preparation method of the viscose fiber compounded by the temperature-adjusting microcapsule and the graphene comprises the following steps: mixing 9 parts (by weight) of temperature-adjusting microcapsule, graphene powder: 2 parts of the composite viscose fiber is added into 1000 parts of viscose spinning coagulating bath containing 8.5 percent of cellulose, the mixture is stirred uniformly by strong force, and the subsequent grinding, dissolution, ripening, defoaming, ripening, secondary filtration, degassing in a degassing tank and spinning in a spinning machine are finished according to the conventional process, and the composite viscose fiber is processed into the temperature-regulating microcapsule and graphene composite viscose fiber with the length of 38mm, the fineness of 1.25D and the crimp of 5 pieces/cm according to the requirement.
The invention has the beneficial effects that the phase-change material microcapsule is prepared by adopting a complex phase double-layer coating method, then the prepared phase-change microcapsule, the graphene material and the adhesive are mixed according to a certain proportion, a coagulating bath of the viscose fiber by a two-bath method is added, and then the viscose fiber compounded by the temperature-adjusting microcapsule and the graphene is prepared by a series of conventional silk making processes. DSC test results of the prepared temperature-regulating microcapsule and graphene composite viscose fiber show that the temperature regulating range of the phase-change temperature-regulating graphene fiber is 20.38-30.13 ℃, the peak value is 25.97 ℃, the solidification temperature range is 19.25-22.76 ℃, the melting heat of the phase-change temperature-regulating graphene fiber is 51.32J/g, the solidification heat is 42.19J/g, and the fiber isMass specific resistance of 7.95 × 107Omega, the enthalpy of phase change is 41.49J/g, the bacteriostasis rates of staphylococcus aureus, escherichia coli and candida albicans are 99.2%, 99.6% and 97.8%, and the ultraviolet shielding rate UPF of the prepared plain weave fabric is improved by 78% compared with that of a common viscose fiber without the phase change microcapsule and the graphene. Has good antistatic, antibacterial and uvioresistant performances. After 50 times of washing, the performance reduction of each type is less than 5 percent.

Claims (8)

1. A preparation method of a temperature-adjusting microcapsule and graphene compounded viscose fiber is characterized by comprising the following steps: adding 8-10 parts of temperature-adjusting microcapsules and 1-3 parts of graphene powder into 1000 parts of viscose spinning coagulating bath containing 8-9% of cellulose according to the weight ratio, uniformly stirring, then grinding, dissolving, ripening, defoaming, ripening, filtering twice, degassing in a degassing tank, spinning by a spinning machine, and processing into viscose fiber compounded by the temperature-adjusting microcapsules and the graphene with certain length, titer and curling according to the requirements.
2. The preparation method of viscose fiber compounded by temperature-regulating microcapsules and graphene according to claim 1, wherein the temperature-regulating microcapsules comprise a core material, the core material is coated with a first shell material, the first shell material is coated with a second shell material, and the viscose fiber compounded by the temperature-regulating microcapsules and graphene specifically comprises the following components in percentage by mass: the core material is waste swill recovered animal and plant modified grease: 50-60%, the first layer of shell material is gelatin: 10-20% of the second layer of shell material, and 20-35% of the aqueous polyurethane solution.
3. The preparation method of the viscose fiber compounded by the temperature-adjusting microcapsules and the graphene according to claim 2, wherein the preparation method of the temperature-adjusting microcapsules specifically comprises the following steps:
step 1, preparing waste swill and recovering animal and plant modified grease;
step 2, coating the animal and plant modified grease recovered from the waste swill prepared in the step 1 in gelatin by adopting a coating method to obtain gelatin-coated modified grease microcapsule particles;
and 3, coating the gelatin-coated modified grease microcapsule particles obtained in the step 2 in an aqueous polyurethane solution by adopting a coating method to form temperature-regulating microcapsule particles.
4. The preparation method of the viscose fiber compounded by the temperature-adjusting microcapsule and the graphene according to claim 3, wherein the step 1 specifically comprises: the preparation method of the animal and plant modified grease recovered from waste swill comprises the following steps: recovering the waste swill from the animal and plant modified grease, introducing hydrogen into a closed reaction kettle, and carrying out hydrogenation treatment for 6-8 hours at the temperature of 120-130 ℃ and the pressure of 1.8-2.0MPa to obtain the animal and plant modified grease recovered from the waste swill.
5. The preparation method of the viscose fiber compounded by the temperature-adjusting microcapsule and the graphene according to claim 3, wherein the step 2 specifically comprises: adding the animal and plant modified grease recovered from the waste swill prepared in the step 1 into 10-20% gelatin solution, shearing at high speed for 20-30 minutes under the condition of 16000-.
6. The method for preparing the viscose fiber compounded by the temperature-regulating microcapsule and the graphene according to claim 5, wherein the weight ratio of the animal and plant modified grease recovered from the waste swill to the 10-20% gelatin solution is as follows: 5-6: 10.
7. the preparation method of the viscose fiber compounded by the temperature-adjusting microcapsule and the graphene according to claim 3, wherein the step 3 specifically comprises:
adding the gelatin-coated modified grease microcapsule particles into 10-20% aqueous polyurethane solution, shearing at high speed for 15-20 minutes under the conditions of 16000 and 18000 revolutions per minute, and carrying out vacuum concentration and drying for 6-8 hours under the stirring state to form the temperature-regulating microcapsule particles.
8. The preparation method of the viscose fiber compounded by the temperature-adjusting microcapsule and the graphene according to claim 7, wherein the weight ratio of the gelatin-coated modified oil microcapsule particles to the 10-20% aqueous polyurethane solution is as follows: 6-8:10.
CN202010506609.1A 2020-06-05 2020-06-05 Preparation method of temperature-adjusting microcapsule and graphene compounded viscose fiber Pending CN111676536A (en)

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Application publication date: 20200918