CN107354527B - A kind of preparation method of speed heat warm-keeping cellulose fiber - Google Patents

A kind of preparation method of speed heat warm-keeping cellulose fiber Download PDF

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Publication number
CN107354527B
CN107354527B CN201710691878.8A CN201710691878A CN107354527B CN 107354527 B CN107354527 B CN 107354527B CN 201710691878 A CN201710691878 A CN 201710691878A CN 107354527 B CN107354527 B CN 107354527B
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speed heat
slurry
fiber
added
cellulose
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CN107354527A (en
Inventor
刘长军
马君志
秦翠梅
李昌垒
刘乐
王东
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Weifang Xinlong Biomaterials Co Ltd
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Hengtian Hailong (weifang) New Materials Co Ltd
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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)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

The present invention provides a kind of preparation method of speed heat warm-keeping cellulose fiber, addition speed heat material and thermal control material before cellulose fiber spinning forms.Pure fibers spinning prepared by the present invention can have the function of heat generating and retention, can also be widely used as the clothing of underwear, nightwear, sweat shirt, socks etc. with human body close contact, processability is excellent, widely used with other fiber blends;Prepared fiber can not only quickly generate thermal sensation, and have the function of adjusting temperature.Conventional cellulosic fibers and speed heat warm-keeping cellulose fiber are subjected to thermal property contrast test, referring to light absorption thermal insulation property test method (BQE A 036-2011), it was found that the speed heat warm-keeping cellulose fiber by the technical program preparation is 5 ~ 16 DEG C higher than temperature in common viscose fiber light irradiation 10min, it is 2 ~ 8 DEG C high in the 10min that turns off the light.

Description

A kind of preparation method of speed heat warm-keeping cellulose fiber
Technical field
The present invention relates to a kind of speed heat warm-keeping cellulose fibers and preparation method thereof, specifically, being related to one kind with fiber Cellulose fiber is matrix, and will there is the slurry of fever, heat-preserving function to be added in spinning solution, has speed through what wet spinning was prepared into The health fiber of hot heat-preserving function, belongs to textile technology field.
Background technique
Keep warm is the critical function of water clothes.Traditional insulation garment is to prevent the heat losses of body from being Main, weakly people needs to wear more thick and heavy clothing to keep warm, and is unfavorable for the comfortable and movable of body.Heat can actively be generated And frivolous warming clothes, it is to be greatly improved to traditional textile.
Thermal fiber has positive thermal insulation property, can absorb extraneous heat, preferably warms up sense to human body.It is representative Thermal fiber has sunlight thermal fiber, phase-change energy-storage fibre, hygroscopic heating fibers etc..Sunlight thermal fiber is will to absorb the sun The luminous energy and material that can be converted into thermal energy is added in fiber, can give off heat under the action of solar thermal energy and can reflect wave The fiber of long longer far infrared.Hygroscopic heating fibers are the sensitive responses by moisture and extraneous pressure change, are people Body provides the fiber of comfortable moist heat.Phase-change energy-storage fibre be using fiber it is basic in suction of the phase change medium to heat It receives, discharge to reach a kind of fiber with temperature adjustment function for keeping ambient stable.The Heating mechanism of different heat fiber It is different, but can all increase the warmth retention property of clothing.But single heat generating fiber is because of the limitation of material itself, and heating effect is by ring The factors such as border, exothermic material restrict, and exist and need certain condition excitation or the unendurable disadvantage of heating effect.
102660792 B of Chinese invention patent CN provides the technique that a kind of solvent method prepares sunlight heat accumulation thermal fiber, Chinese invention patent Publication No. " CN 101580969 " provides a kind of method that viscose process prepares heat accumulation thermal fiber.This two A patent is all that zirconium carbide is added in cellulose solution, carries out blending wet spinning.Although having warming effect, need Heat, high-energy ray of the nano-zirconium carbide powder energy absorbing wavelength less than 2 μm, and reflection wavelength are absorbed under given conditions Low energy ray greater than 2 μm can generate heat under sunlight irradiation, cannot store heat, and the ability without cooling and temperature adjustment.
102605614 B of Chinese invention patent CN, which is provided, a kind of is incorporated in one for phase change energy storage technology and exothermic material The bidirectional temp regulation fiber risen, this material can active heat production, and can keep the temperature.Although the fiber has preferable warmth retention property, Starching that the patent is mentioned, pad, be sprayed, paint-on technique belongs to the final finishing technology of fiber, exothermic material easily falls off from surface layer, The blended weave for various other fibers that the patent is mentioned, needs to be processed into different clad structures, can be only achieved knitting for fever Object, complex process.
Summary of the invention
The problem to be solved in the present invention is the deficiency for the above present Research and technology, provide it is a kind of can actively generate heat, Exothermic material and thermal control material are evenly distributed on every fiber by the preparation method of the cellulose fibre with temperature adjustment function, Prepared fiber quickly generates thermal sensation, and speed heat warm-keeping cellulose fiber is higher by 5 than temperature in common viscose fiber light irradiation 10min It is ~ 16 DEG C, 2 ~ 8 DEG C high in the 10min that turns off the light;And have the function of adjusting temperature, warming effect is lasting.
Technical scheme is as follows:
The speed heat warm-keeping cellulose fiber, is to prepare cellulose solution by primary raw material of pulp, in cellulose Speed heat material and thermal control material are added before fiberizing, and the fiber with warming effect is prepared by wet spinning technology.
The speed heat material is selected from the material that can emit infrared function, is preferably Tourmaline, bamboo charcoal, graphite The compound of alkene, tin oxide and antimony oxide;
IV group 4 transition metal element compound material of the periodic table of elements also can be selected in the speed heat material, is preferably carbonization Zirconium, zirconium oxide;
The speed heat material can be one or more mixtures of above-mentioned speed heat material, the addition in cellulose solution Amount is 0.5~8wt% of the effective content to alpha cellulose;
The speed heat material will first be prepared into the slurry that mass fraction is 8~20%, and preparation process will be stirred adequately It mixes, preparation process needs to be added dispersing agent, thickener, 2 μm of < of the slurry partial size D90 of preparation;
The speed heat slurry, preparation process are preferred are as follows: deionized water is added, opens blender, dispersing agent is added, speed is added Hot powder, stirring are added thickener after 20-30 minutes, are persistently stirred to D90 less than 2 μm.
The dispersing agent of the speed heat slurry is preferably neopelex, calgon, polyethylene glycol, silicon One of alkane coupling agent, additional amount are 0.5~3wt% of slurry;
For the stability for keeping speed heat slurry, add thickener in decentralized system, additive amount be slurry 0.5~ 1.5wt% is preferably sodium alginate, one of microcrystalline cellulose, hydroxyethyl cellulose.
The thermal control material is phase-change microcapsule slurry, and 2 μm of the partial size D90 < of slurry, additive amount is effective content pair 5~10wt% of alpha cellulose;
The adding method are as follows: speed heat material and thermal control material are added in dissolution glue and pass through after stirring Sufficient mechanical stirring, then through mixing, filtering, deaeration, speed heat thermal fiber is prepared through wet spinning.
Speed heat powdery pulp is preferably added to blender by the addition manner of the speed heat material and thermal control material In, after ten minutes, phase-change microcapsule slurry is added in stirring, continue stirring 1.5 hours, Blend rubber again through mixing, filtering, deaeration, Spin out speed heat warm-keeping cellulose fiber.
Addition manner can also are as follows: injection is added to before being sufficiently stirred speed heat material and thermal control material, being spun after deaeration Co-blended spinning is carried out in spinning glue, prepares speed heat thermal fiber.
It uses n-octadecane as the material of phase transformation capsule capsule-core, is undergone phase transition at 28 DEG C or so, use n-eicosane as phase The core materials for becoming capsule, undergo phase transition at 37 DEG C or so, unused phase transformation capsule-core can be selected according to uses of fabric, to weaving The warming temperature of product is adjusted, intelligent control material temperature.
Innovative point of the invention is not only to joined exothermic material, but also joined the phase that can be stored heat, discharge heat Become capsule, makes up homogenous material and generate heat problem subject to conditions, it can be achieved that function that is preferably warming and adjusting temperature.
It not only joined exothermic material in the present invention, but also joined phase transformation capsule, which can be with environment temperature Thermal discharge is inhaled in the lifting of degree.When the heat that environment temperature increases or exothermic material issues is high, phase transformation capsule can absorb heat, when Environment temperature is low or exothermic material adstante febre, phase transformation capsule can not discharge heat, textile made still to have warming effect.
By adopting the above-described technical solution, compared with the prior art, the invention has the following beneficial effects:
1, pure fibers prepared by the present invention spinning can have the function of heat generating and retention, can also with other fiber blends, It is widely used as the clothing of underwear, nightwear, sweat shirt, socks etc. with human body close contact, processability is excellent, and purposes is wide It is general.
Prepared fiber can not only quickly generate thermal sensation, and have the function of adjusting temperature.
Conventional cellulosic fibers and speed heat warm-keeping cellulose fiber are subjected to thermal property contrast test, are protected referring to light absorption Warm method for testing performance (BQE A 036-2011), discovery is by the speed heat warm-keeping cellulose fiber of the technical program preparation than common Temperature is 5 ~ 16 DEG C high in viscose rayon light irradiation 10min, 2 ~ 8 DEG C high in the 10min that turns off the light.
2, fiber prepared by the present invention is reproducible green fiber cellulose fiber, not only warming, but also moisture absorption is ventilative Property is good, comfortable and easy to wear.
3, the fiber prepared through the invention not only have actively generate heat material, also added be adjustable temperature phase transformation it is micro- Capsule, as the variation of temperature is absorbed heat, heat release, by the temperature control of fiber in the temperature for being suitble to human body, Single Fiber is not Need it is blended, do not need final finishing coating exothermic mixture, so that it may have the function of heat generating and retention, and whole fiber is uniformly distributed Fever auxiliary agent, solve the problems, such as that single exothermic material warming effect is influenced by environment or shooting condition, and the fiber Intelligence adjusts temperature function, and fabric is made to have better wearability.
4, Tourmaline, bamboo charcoal, graphene exothermic material that the present invention adds not only generate thermal sensation, but also have excitation negative Ion function, antibacterial functions, are more suitable for human health.
Specific embodiment
The following describes the present invention in detail with reference to examples.
A kind of preparation method of the speed heat warm-keeping cellulose fiber of embodiment 1
The following steps are included:
(1) speed heat slurry is prepared
Speed heat powder Tourmaline, zirconium carbide are configured to the slurry that mass fraction is 8% respectively.
Preparation method are as follows: deionized water is added in blend tank, opens blender, 1% dodecyl benzene sulfonic acid is added Sodium, is added speed heat powder Tourmaline or zirconium carbide, and 1% sodium alginate is added after twenty minutes, is persistently stirred to D90 less than 2 for stirring μm, respectively be made mass fraction be 8% Tourmaline speed heat slurry, mass fraction be 8% zirconium carbide speed heat slurry.
Above-mentioned neopelex, Tourmaline, zirconium carbide, sodium alginate additional amount be slurry relative to preparation Material.
(2) speed heat powdery pulp and the mixing of phase-change microcapsule slurry
Carbonization by effective component to the Tourmaline, effective component of viscose glue alpha cellulose 3% to viscose glue alpha cellulose 1% Zirconium speed heat slurry is added in blender, and after ten minutes, phase transformation of the effective component to viscose glue alpha cellulose 5% is added in stirring Microcapsules slurry continues stirring 1.5 hours.
(3) co-blended spinning
Blend rubber spins out speed heat warm-keeping cellulose fiber through some column processes such as mixing, filtering, deaeration again.
A kind of preparation method of the speed heat warm-keeping cellulose fiber of embodiment 2
The following steps are included:
(1) speed heat slurry is prepared
Speed heat powder bamboo charcoal, zirconium carbide are configured to the slurry that mass fraction is 20% respectively.
Preparation method are as follows: deionized water is added in blend tank, opens blender, 3% silane coupling agent is added, is added Speed heat powder is added 0.5% microcrystalline cellulose, is persistently stirred to D90 less than 2 μm after stirring 30 minutes;Quality point is made respectively Count the bamboo charcoal speed heat slurry for 20%, the zirconium carbide speed heat slurry that mass fraction is 20%;
Above-mentioned silane coupling agent, microcrystalline cellulose, bamboo charcoal, zirconium carbide additional amount be slurry relative to preparation.
(2) speed heat powdery pulp and the mixing of phase-change microcapsule slurry
Carbonization by effective component to the bamboo charcoal, effective component of viscose glue alpha cellulose 5% to viscose glue alpha cellulose 0.5% Zirconium speed heat slurry is added in blender, and it is micro- to the phase transformation of viscose glue alpha cellulose 8% that effective component is added in stirring after ten minutes Capsule slurry continues stirring 1.5 hours.
(3) co-blended spinning
Blend rubber spins out speed heat warm-keeping cellulose fiber through some column processes such as mixing, filtering, deaeration again.
A kind of preparation method of the speed heat warm-keeping cellulose fiber of embodiment 3
The following steps are included:
(1) speed heat slurry is prepared
Compound (mass ratio is 1:1), the zirconium carbide of speed heat powder tin oxide and antimony oxide are configured to quality respectively The slurry that score is 15%.
Preparation method are as follows: deionized water is added in blend tank, opens blender, 2% polyethylene glycol is added, speed is added 1% hydroxyethyl cellulose is added in hot powder after stirring 30 minutes, be persistently stirred to D90 less than 2 μm, mass fraction is made respectively The zirconium carbide speed heat slurry that tin oxide and antimony oxide speed heat slurry, mass fraction for 15% are 15%.
Above-mentioned polyethylene glycol, hydroxyethyl cellulose, tin oxide and antimony oxide, zirconium carbide additional amount be relative to preparation Slurry.
(2) speed heat powdery pulp and the mixing of phase-change microcapsule slurry
Effective component adds the tin oxide of viscose glue alpha cellulose 1.5% and the compound of antimony oxide, stirring after ten minutes Enter effective component to the phase-change microcapsule slurry of viscose glue alpha cellulose 8%, after continuing stirring 1.5 hours, Blend rubber is again through mixed Some column processes such as conjunction, filtering, deaeration reach spinning, by prepared zirconium carbide slurry through filtering, deaeration, by effective component pair Viscose glue alpha cellulose 2% is added in spinning glue by injecting systems before spinning.
(3) co-blended spinning
Spin out speed heat warm-keeping cellulose fiber.
Unless specifically indicated, percentage of the present invention is mass percent, and the ratio is mass ratio Example.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention, Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features. All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention Within protection scope.

Claims (2)

1. a kind of preparation method of speed heat warm-keeping cellulose fiber, it is characterised in that: the addition before cellulose fiber spinning forms Speed heat material and thermal control material;
The speed heat material is selected from the IV group 4 transition metal element of material or the periodic table of elements that can emit infrared function Close the one or more of object material;Additive amount of the speed heat material in cellulose solution is effective content to alpha cellulose 0.5~8wt%;
It is described that there is the material that can emit infrared function, it is Tourmaline, bamboo charcoal, graphene, tin oxide and antimony oxide compound One of or it is a variety of;
The IV group 4 transition metal element compound material of the periodic table of elements is zirconium carbide, zirconium oxide one or two;
The speed heat material will first be prepared into the speed heat slurry that mass fraction is 8~20%;
The thermal control material is phase-change microcapsule;The phase-change microcapsule is first prepared into phase-change microcapsule slurry, slurry 2 μm of partial size D90 <, additive amount of the phase-change microcapsule in cellulose solution be effective content to the 5 of alpha cellulose~ 10wt%;
The speed heat slurry, preparation process are as follows: deionized water is added, opens blender, dispersing agent is added, speed heat powder is added, Thickener is added after 20-30 minutes in stirring, is persistently stirred to D90 less than 2 μm;
The dispersing agent is neopelex, calgon, polyethylene glycol, and one of silane coupling agent is added Amount is 0.5~3wt% of slurry;
The thickener be one of sodium alginate, microcrystalline cellulose, hydroxyethyl cellulose, additive amount be slurry 0.5~ 1.5wt%;
The addition manner of the speed heat material and thermal control material is speed heat slurry and phase-change microcapsule slurry through stirring Afterwards, it is added in dissolution glue through sufficient mechanical stirring, then through mixing, filtering, deaeration, it is warming to prepare speed heat through wet spinning Fiber;Or injection is added in spinning glue before being sufficiently stirred speed heat slurry and phase-change microcapsule slurry, being spun after deaeration Co-blended spinning is carried out, speed heat thermal fiber is prepared.
2. a kind of preparation method of speed heat warm-keeping cellulose fiber according to claim 1, it is characterised in that:
The addition manner of the speed heat material and thermal control material, speed heat powdery pulp is added in blender, stirs 10 points Phase-change microcapsule slurry is added in Zhong Hou, continues stirring 1.5 hours, and Blend rubber through mixing, filtering, deaeration, spins out speed heat guarantor again Warm cellulose fibre.
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CN108499497A (en) * 2018-04-18 2018-09-07 济南圣泉集团股份有限公司 A kind of graphene microcapsules, intelligent temperature adjusting fiber and preparation method thereof
CN108816164A (en) * 2018-06-01 2018-11-16 罗莱生活科技股份有限公司 A kind of Sophora alopecuroide and anise extract microcapsules, microcapsules compound system, regenerated celulose fibre and preparation method thereof
CN110284209A (en) * 2019-06-28 2019-09-27 厦门安踏体育用品有限公司 Multi-functional viscose rayon, preparation method and the fabrics such as a kind of temperature regulation, antibacterial
CN110528097B (en) * 2019-07-31 2021-03-30 天津工业大学 Photothermal conversion, heat storage and temperature regulation cellulose fiber and preparation method thereof
CN114763629A (en) * 2021-05-24 2022-07-19 上海九裕纺织科技有限公司 Fabric with heating function and preparation method thereof
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CN102839440A (en) * 2012-09-24 2012-12-26 成都丽雅纤维股份有限公司 Cotton, wood and bamboo composite pulp phase-change microcapsule viscose and preparation method thereof
CN104831388A (en) * 2015-04-30 2015-08-12 湖州珠力纳米材料科技开发有限公司 Preparation method of temperature regulating fiber
CN104947220A (en) * 2015-07-22 2015-09-30 湖南莎丽袜业股份有限公司 Preparation method of flax-viscose-mint heat-insulating fiber and sock
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