CN107299405A - A kind of preparation method of hollow speed heat warm-keeping cellulose fiber - Google Patents

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

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Publication number
CN107299405A
CN107299405A CN201710691739.5A CN201710691739A CN107299405A CN 107299405 A CN107299405 A CN 107299405A CN 201710691739 A CN201710691739 A CN 201710691739A CN 107299405 A CN107299405 A CN 107299405A
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China
Prior art keywords
speed heat
preparation
slurry
cellulose fiber
keeping
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CN201710691739.5A
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Chinese (zh)
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CN107299405B (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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Constant Day Dragon (weifang) New Material 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
    • 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
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties

Abstract

The present invention provides a kind of preparation method of hollow speed heat warm-keeping cellulose fiber, include the preparation of speed heat slurry, add and cause the gentle forming agent of empty agent, co-blended spinning, fiber prepared by the present invention is post-treated, drying obtains hollow speed heat cellulose fibre, degree of hollowness is 20 50%, conventional cellulosic fibers and hollow speed heat warm-keeping cellulose fiber is carried out into thermal property contrast test, with reference to light absorbs heat-insulating property test method(BQE A 036‑2011), it is found that the temperature in light irradiation 10min is high 5 ~ 15 DEG C than common viscose fiber by the speed heat warm-keeping cellulose fiber of the technical program preparation, it is high 4 ~ 7 DEG C in the 10min that turns off the light.

Description

A kind of preparation method of hollow speed heat warm-keeping cellulose fiber
Technical field
The present invention relates to a kind of hollow speed heat warm-keeping cellulose fiber and preparation method thereof, specifically, be related to it is a kind of with Cellulose fibre is matrix, the slurry with heating, heat-preserving function is added in spinning solution, the tool being prepared into through wet spinning There are hollow structure, the health fiber of speed heat heat-preserving function, belong to textile technology field.
Background technology
Traditional insulation garment outward appearance is thick and heavy, fluffy too fat to move, not only lacks aesthetic feeling, and be unfavorable for the activity of body.With The improvement of people's living standards and the progress of science and technology, requirement more and more higher of the people to clothes, not only comfortably, and attractive in appearance It is generous.Warming is one of major function of clothes, and light, good warmth retention effect dress material can not only resist cold, and meet People are to beautiful pursuit, therefore demand is increasing.
Thermal fiber is divided to actively warming and passive warming two kinds.Passive thermal fiber can only prevent or reduce merely Studies of Human Body Heat Amount is scattered and disappeared, and light passive thermal fiber is based on doughnut, and hollow layer can store part still air, and barrier is extraneous to tremble with fear It is cold.Positive thermal fiber is will to be added with the functional material that can absorb extraneous electric energy, chemical energy, biological energy source, solar energy etc. Into fiber.Research at present on thermal fiber is more, but by actively it is warming and it is passive it is warming combine have it is dual The cellulose fibre research of warming effect is less.
The B of Chinese invention patent CN 102660792 provide the technique that a kind of solvent method prepares sunlight heat accumulation thermal fiber, " CN 101580969 " provides a kind of method that viscose process prepares heat accumulation thermal fiber to Chinese invention patent Publication No..This two Individual patent is all that zirconium carbide is added in cellulose solution, carries out blending wet spinning.Although with warming effect, needing Heat is absorbed under given conditions, and nano-zirconium carbide powder energy absorbing wavelength is less than 2 μm of high-energy ray, and reflection wavelength Low energy ray more than 2 μm, can generate heat, it is impossible to store heat under sunshine irradiation.
The B of Chinese invention patent CN 104389043 provide a kind of hollow warming heat generating fiber of polycaprolactam and its added Work method, is that, by polycaprolactam heating master batch and polycaprolactam section progress co-blended spinning, the hollow heating prepared gathers Caprolactam preoriented yarn carries out fluffy crimpiness processing and prepares final thermal fiber.Although the fiber has preferable guarantor Warm property, but belong to synthetic fibers, sucting wet air permeability is poor, wears uncomfortable.The A of Chinese invention patent CN 101089256 are provided A kind of preparation method of doughnut cellulose fiber, although the degree of hollowness of preparation is higher, but the fiber can only have passive warming effect Really, it is impossible to carry out active heat generating and retention.
The content of the invention
The problem to be solved in the present invention is that there is provided a kind of hollow speed heat is warming for above present Research and technology not enough The preparation method of fiber, using pulp as primary raw material, is prepared into uniformly by the process such as being disperseed, being ground to speed heat material Slurry, is added in cellulose solution through spinning preceding injecting systems, hollow speed heat thermal fiber is prepared by wet spinning technology Cellulose fiber, to realize following goal of the invention:
(1)Fiber prepared by the present invention, degree of hollowness reaches 20-50%;
(2)The present invention prepares speed heat warm-keeping cellulose fiber, and than common viscose fiber, the temperature in light irradiation 10min is high 5 ~ 15 DEG C, Turn off the light high 4 ~ 7 DEG C in 10min.
The technical scheme that the present invention takes is as follows:
Described hollow speed heat warm-keeping cellulose fiber, is to prepare in cellulose solution, cellulose solution to add with common process Empty agent and slow forming agent are caused, by injecting the speed heat slurry after decorum addition filtering, deaeration before spinning, through wet spinning, fiber exists Hollow structure is generated in coagulating bath, then hollow speed heat fiber is prepared in post-treated, drying.
The speed heat material is selected from the material with the emitting far-infrared function of energy, the group 4 transition metal of the periodic table of elements IV member Plain compound-material is preferably Tourmaline, zirconium carbide, titanium carbide, graphene;
Described speed heat material can be that the addition in one or more mixtures of above-mentioned speed heat material, cellulose solution is 0.5~3wt % of the effective content to alpha cellulose;
Described speed heat material will first be prepared into the slurry that mass fraction is 8~20%, and preparation method is:It is being sufficiently stirred for condition Under, dispersant is added in deionized water, nano level speed heat powder is then slowly added into, and adds defoamer, 1500~ Disperse 10~30 minutes under 3000rpm, add grinder and be ground to 2 μm of slurry particle diameter D90 <;
The dispersant of described speed heat slurry is preferably neopelex, calgon, polyethylene glycol, and silane is even Join one kind in agent, addition is 0.5~1.5wt% of slurry;
To keep the stability of speed heat slurry, thickener is added in decentralized system, addition is 0.5~1.5wt% of slurry, Preferably it is sodium alginate, microcrystalline cellulose.
The addition of the defoamer is the 3-4.5 ‰ of slurry.
The preparation method of described doughnut is:Addition causes empty agent in cellulose solution, and addition is the 5 of alpha cellulose ~10wt%, adds slow forming agent in the cellulose solution of dissolving, and addition is 2~3wt% of alpha cellulose;
Described to cause empty agent to be preferably sodium carbonate, sodium acid carbonate, slow forming agent is preferably polyethylene glycol, fatty amine;
The preparation method, including co-blended spinning, are filtered to the speed heat slurry of preparation with filter, are by being injected before spinning after deaeration System is added in spinning glue, and the addition of speed heat slurry is 0.5-3.0 of the effective content to alpha cellulose of speed heat material wt%;
The spinning, 28-40 DEG C of coagulation bath temperature, sulfuric acid 90-95g/l, sodium sulphate 320-330g/l, zinc sulfate 35-40g/l.
Positive heating system two of the present invention by the hollow structure with passive warming effect with adding exothermic material heating Person combines, and not only adds exothermic material, and makes hollow, and hollow structure can include substantial amounts of still air, not only Extraneous cold can be separated, and it is more slim and graceful, warming effect can be increased.
By adopting the above-described technical solution, the present invention has the advantages that compared with prior art:
(1)Fiber prepared by the present invention is post-treated, drying obtains hollow speed heat cellulose fibre, and degree of hollowness is 20-50%, will Conventional cellulosic fibers and hollow speed heat warm-keeping cellulose fiber carry out thermal property contrast test, with reference to light absorbs heat-insulating property Test method(BQE A 036-2011), it is found that the speed heat warm-keeping cellulose fiber prepared by the technical program is more fine than common viscose glue Dimension temperature in light irradiation 10min is high 10 ~ 15 DEG C, high 4 ~ 7 DEG C in the 10min that turns off the light.
(2)The hollow speed heat cellulose fibre prepared by the present invention, with the addition of the material that can actively generate heat, in also having Hollow structure, therefore have actively warming and passive warming two kinds of effects, it can greatly improve the thermal property of fiber.Hollow structure makes Dress material is slimmer and more graceful, warming, good permeability, and dyeability is good, improves the wearability of textile.
Speed heat slurry addition prepared by the present invention is few, and good dispersion is not precipitated, and granularity is small, is conveniently added to cellulose In solution, heating effect is obvious.
Embodiment
With reference to embodiment, the present invention is described in detail.
A kind of preparation method of hollow speed heat warm-keeping cellulose fiber of embodiment 1
Comprise the following steps:
(1)The preparation of speed heat slurry:
Under the conditions of being sufficiently stirred for, 0.5wt% neopelex is added in deionized water, it is slow after being uniformly dispersed 0.5wt% sodium alginate is added, the nano level zirconium carbides of 8wt% are then slowly added into, 3 ‰ wt% defoamer is added, Disperse 30 minutes under 1500rpm, add grinder and grind 5 hours, slurry particle diameter D90=1.564 are detected with laser fineness gage μm。
Above-mentioned slow, slowly criterion sees that conglomeration just etc. stirs to open and is further continued for adding to be slowly added to.
Above-mentioned dispersant, thickener, defoamer, the addition of speed heat material are calculated relative to slurry.
(2)Add and cause the gentle forming agent of empty agent
Cellulose solution is prepared with common process, the carbonic acid to alpha cellulose 5wt% is added in the cellulose solution after yellow Sodium, adds fatty amine as slow forming agent, addition is the 0.5wt% to alpha cellulose.
(3)Co-blended spinning
The speed heat slurry of preparation is filtered with filter, is added to after deaeration by spinning preceding injecting systems in spinning glue, addition is 0.5 wt% of the effective content to alpha cellulose.
The fiber of preparation is post-treated, to obtain degree of hollowness be 26% for drying, than conventional cellulosic fibers illumination 10min temperature It is high 10 DEG C, high 4 DEG C of the 10min that turns off the light hollow speed heat cellulose fibre.
A kind of preparation method of hollow speed heat warm-keeping cellulose fiber of embodiment 2
Comprise the following steps:
(1)The preparation of speed heat slurry
Under the conditions of being sufficiently stirred for, 1.0wt% polyethylene glycol is added in deionized water, is slowly added to after being uniformly dispersed 1.0wt% microcrystalline cellulose, is then slowly added into the nano level graphenes of 10wt%, the nano level titanium carbides of 5wt%, adds 3.5 ‰ wt% defoamer, disperses 40 minutes under 2000rpm, adds grinder and grinds 8 hours, is examined with laser fineness gage Survey slurry particle diameter D90=1.428 μm.
Above-mentioned slow, slowly criterion sees that conglomeration just etc. stirs to open and is further continued for adding to be slowly added to.
Above-mentioned dispersant, thickener, defoamer, the addition of speed heat material are calculated relative to slurry.
(2)Add and cause the gentle forming agent of empty agent
Cellulose solution is prepared with common process, the carbonic acid to alpha cellulose 8wt% is added in the cellulose solution after yellow Sodium, adds polyethylene glycol as slow forming agent, addition is the 1.0wt% to alpha cellulose.
(3)Co-blended spinning
The speed heat slurry of preparation is filtered with filter, is added to after deaeration by spinning preceding injecting systems in spinning glue, addition is 1.0wt% of the effective content to first kind fiber.
The fiber of preparation is post-treated, to obtain degree of hollowness be 38% for drying, higher by 12 than conventional cellulosic fibers illumination 10min temperature DEG C, the 10min that turns off the light is high 5 DEG C.
A kind of preparation method of hollow speed heat warm-keeping cellulose fiber of embodiment 3
Comprise the following steps:
(1)The preparation of speed heat slurry
Under the conditions of being sufficiently stirred for, 1.5wt% calgon is added in deionized water, is slowly added to after being uniformly dispersed 1.5wt% microcrystalline cellulose, is then slowly added into the nano level zirconium carbides of 10wt%, the nano level titanium carbides of 10wt%, adds 4.5 ‰ wt% defoamer, disperses 60 minutes at 3,000 rpm, adds grinder and grinds 8 hours, is examined with laser fineness gage Survey slurry particle diameter D90=1.822 μm.
Above-mentioned slow, slowly criterion sees that conglomeration just etc. stirs to open and is further continued for adding to be slowly added to.
Above-mentioned dispersant, thickener, defoamer, the addition of speed heat material are calculated relative to slurry.
(2)Add and cause the gentle forming agent of empty agent
Cellulose solution is prepared with common process, the bicarbonate to cellulose 10wt% is added in the cellulose solution after yellow Sodium, the polyethylene glycol for adding 1.5 wt% is used as slow forming agent.
(3)Co-blended spinning
The speed heat slurry of preparation is filtered with filter, is added to after deaeration by spinning preceding injecting systems in spinning glue, addition is 3.0wt% of the effective content to first kind fiber.
The fiber of preparation is post-treated, to obtain degree of hollowness be 46% for drying, than conventional cellulosic fibers illumination 10min temperature High 15 DEG C, the 10min that turns off the light is high 7 DEG C.
Unless specifically indicated, percentage of the present invention, is mass percent, and described ratio is mass ratio Example.
Finally it should be noted that:The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, Although the present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art, it still may be used To be modified to the technical scheme described in foregoing embodiments, or equivalent substitution is carried out to which part technical characteristic. Within the spirit and principles of the invention, any modification, equivalent substitution and improvements made etc., should be included in the present invention's Within protection domain.

Claims (9)

1. a kind of preparation method of hollow speed heat warm-keeping cellulose fiber, it is characterised in that:Include the preparation of speed heat slurry, add Cause the gentle forming agent of empty agent, co-blended spinning.
2. a kind of preparation method of hollow speed heat warm-keeping cellulose fiber according to claim 1, it is characterised in that:It is described The preparation of speed heat slurry, under the conditions of being sufficiently stirred for, adds dispersant, is then slowly added into nano level speed in deionized water Hot material powder, adds defoamer, disperses 10~30 minutes under 1500~3000rpm, adds grinder and is ground to slurry grain 2 μm of footpath D90 <, are prepared into the slurry that mass fraction is 8~20%.
3. a kind of preparation method of hollow speed heat warm-keeping cellulose fiber according to claim 2, it is characterised in that:It is described Speed heat material is selected from material, the group 4 transition metal element compound material of the periodic table of elements IV with the emitting far-infrared function of energy One or more, the addition of the speed heat material is 0.5~3wt % of the effective content to alpha cellulose.
4. a kind of preparation method of hollow speed heat warm-keeping cellulose fiber according to claim 3, it is characterised in that:It is described Speed heat material, preferably Tourmaline, zirconium carbide, titanium carbide, graphene.
5. a kind of preparation method of hollow speed heat warm-keeping cellulose fiber according to claim 2, it is characterised in that:It is described Dispersant is preferably one kind in neopelex, calgon, polyethylene glycol, silane coupler, and addition is 0.5~1.5wt% of slurry.
6. a kind of preparation method of hollow speed heat warm-keeping cellulose fiber according to claim 2, it is characterised in that:It is described The addition of defoamer is the 3-4.5 ‰ of slurry.
7. a kind of preparation method of hollow speed heat warm-keeping cellulose fiber according to claim 2, it is characterised in that:To protect The stability of speed heat slurry is held, thickener is added in decentralized system, addition is 0.5~1.5wt% of slurry.
8. a kind of preparation method of hollow speed heat warm-keeping cellulose fiber according to claim 1, it is characterised in that:It is described Add and cause the gentle forming agent of empty agent, addition causes empty agent in cellulose solution, and addition is 5~10wt% of alpha cellulose, Slow forming agent is added in the cellulose solution of dissolving, addition is 2~3wt% of alpha cellulose;It is described to cause the empty agent to be preferably Sodium carbonate, sodium acid carbonate, slow forming agent are preferably polyethylene glycol, fatty amine.
9. a kind of preparation method of hollow speed heat warm-keeping cellulose fiber according to claim 1, it is characterised in that:It is described Co-blended spinning, is added in spinning glue to the speed heat slurry of preparation, carries out co-blended spinning.
CN201710691739.5A 2017-08-14 2017-08-14 A kind of preparation method of hollow speed heat warm-keeping cellulose fiber Active CN107299405B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110952218A (en) * 2019-11-28 2020-04-03 江阴龙阳纺织有限公司 Preparation method of nano-enhanced far infrared thermal fabric

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110952218A (en) * 2019-11-28 2020-04-03 江阴龙阳纺织有限公司 Preparation method of nano-enhanced far infrared thermal fabric

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Effective date of registration: 20211227

Address after: 261106 north of Xinsha Road, Guti street, Hanting District, Weifang City, Shandong Province

Patentee after: Weifang Xinlong biomaterials Co.,Ltd.

Address before: 261100 building 89, 1825 Hailong Road, Hanting District, Weifang City, Shandong Province

Patentee before: HENGTIAN HAILONG (WEIFANG) NEW MATERIALS CO.,LTD.