CN105671664B - A kind of temperature adjustment antimicrobial pearl regenerated celulose fibre and preparation method thereof - Google Patents
A kind of temperature adjustment antimicrobial pearl regenerated celulose fibre and preparation method thereof Download PDFInfo
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- CN105671664B CN105671664B CN201510664573.9A CN201510664573A CN105671664B CN 105671664 B CN105671664 B CN 105671664B CN 201510664573 A CN201510664573 A CN 201510664573A CN 105671664 B CN105671664 B CN 105671664B
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Abstract
The present invention relates to a kind of temperature adjustment antimicrobial pearl regenerated celulose fibres and preparation method thereof, and preparation process is：Preparing temperature control pearl microcapsules, --- modulation additive mother liquor --- prepares co-blended spinning liquid --- spinning --- post-processing, obtains temperature adjustment antimicrobial pearl regenerated celulose fibre.The temperature control health care microcapsules of the present invention are blended composite core material made of absorption with paraffin by pearl powder and are made of the wall material that high molecular polymer is constituted；Composite core material and the mass ratio of wall material are 0.3~3: 1；Pearl powder average grain diameter≤1.2 μm；Average grain diameter≤3 μm of microcapsules.The present invention solves the comfortable bad and health-care efficacy during existing product is taken in winter and declines, in process of production since the precipitation of pearl powder causes production efficiency to decline, and cost of material improves and enhance the technical problems such as its antibacterial action.
Description
Technical field
The invention belongs to field of textiles, it is related to a kind of temperature adjustment antimicrobial pearl regenerated celulose fibre and preparation method thereof.
Background technology
Currently, as the improvement of people's living standards, requirement of the consumer for the functionality and comfort of textile is cured
Come higher, wherein antibacterial, the demand of comfort health-care class textile increasingly increase.Regenerated celulose fibre weaves strain using day
Right cellulose and/or cotton linter, a series of chemical fibre after manufacturing procedures are prepared into spinning solution obtained by spinning, made of
Textile product has the characteristic of soft absorption comfortable；Pearl is generally acknowledged rare health products, have beauty treatment skin makeup, anti-aging,
The special effects such as Toxin-Vanquishing of relieving inflammation or internal heat.The exploitation of pearl regenerated cellulose textile enriches comfort health-care class piece market, largely
On meet consumer demand.
In the prior art, pearl viscose fiber (Chinese Patent Application No. 200410067962.5) and antimicrobial pearl viscose glue are fine
It ties up (Chinese Patent Application No. 200710008726), is achieved in terms of realizing the blending technology of pearl powder and viscose rayon prominent
It is broken, it takes textile using all kinds of pearls that the prior art is produced and is received by the market.But in actual production and consumer
In suggestion feedback, there are still deficiencies for the prior art, are embodied in：
In consumer's opinion, since pearl is cold in nature, under the conditions of taking summer, consumer feels that pearl fiber underwear is cool
It is refreshing comfortable, by consistent favorable comment；But when taking in winter, underwear is taken excessively cooler, affects comfort to a certain extent.
Furthermore winter temperature is low, there is the shadow now seen for the trace element release of pearl microparticle and far infrared normal emittance
It rings, directly influences the health-care efficacy of product.
In production, since in " pearl viscose fiber " technology, pearl powder liquid slurry uses water soluble dispersing agent, and
Using distilled water as carrier, therefore in spinning process after addition pearl powder liquid slurry, point of the pearl powder in spinning solution
Dissipate property decline, in high-volume spinning, pearl powder block spinneret orifice the phenomenon that happen occasionally, spinning terminates, it is seen that pearl powder
Body is deposited in the bottom of container；This drawback has seriously affected the production efficiency of pearl fiber.Simultaneously as pearl powder is heavy
It forms sediment, increases the cost of raw material.In addition, in the coagulating bath of rayon spinning, the erosion of sulfuric acid inevitably reduces treasure
The active ingredient of pearl powder.
Furthermore since viscose rayon has good hygroscopicity, at a certain temperature, bacterium and fungi be easy to grow,
Breeding, for human body, the human body for especially suffering from skin allergy easily damages.However the antibacterial action of pearl viscose fiber
It is limited.
In the improved technology of pearl fiber production, " antimicrobial pearl viscose fiber " technology is added in pearl powder mother liquor
Organic antibacterial agent, it is polyalcohol tween, certain journey that correspondingly dispersant, which uses polyether-type nonionic activating agent, carrier,
Dispersibility increases on degree, but does not solve above-mentioned drawback fundamentally.Have in addition, antimicrobial pearl viscose fiber technology uses
Machine antiseptic, compared to inorganic antiseptic, heat resistance is poor, is easy hydrolysis, and the antibacterial term of validity is short.
Invention content
Use temperature control pearl microcapsules and inorganic antiseptic for Additive Production the purpose of the present invention is to provide a kind of
Temperature adjustment antimicrobial pearl regenerated celulose fibre and preparation method thereof, with solve during product is taken in winter it is comfortable it is bad and
Health-care efficacy decline, in process of production since the precipitation of pearl powder causes production efficiency to decline, cost of material improve and
Enhance the technical problems such as its antibacterial action.
To achieve the above object, the present invention can be achieved by the following technical programs：
A kind of preparation method of temperature adjustment antimicrobial pearl regenerated celulose fibre of the present invention, step are：Prepare temperature control pearl
--- modulation additive mother liquor --- prepares co-blended spinning liquid --- spinning --- post-processing, obtains temperature adjustment antimicrobial pearl again microcapsules
Raw cellulose fibre.
The step of preparation temperature control pearl microcapsules of the present invention is：Prepare performed polymer --- prepare pearl powder and paraffin
Composite core material emulsion --- polymerisation film forming --- is washed and drying；
The performed polymer step for preparing is：
Melamine, formalin and distilled water are mixed, pH value is adjusted to 8~9, is warming up to 60~80 DEG C, with 200~
500r/min is mixed slowly to clear viscous shape liquid；
The preparation pearl powder is with paraffin composite core material emulsion step：
At a temperature of 40-50 DEG C, after the paraffin, emulsifier and deionized water of fusing are mixed with high speed 6000~
10000r/min is emulsified, and then with oil bath heating to 90~99 DEG C, pearl powder and dispersant is added, continues with 400~600r/
After min rotating speeds emulsify 10~15min, 30~40 DEG C are cooled to, with weak acid for adjusting pH value to 5~6；
The polymerisation film formation step is：
Pearl powder and paraffin composite core material emulsion are warmed to 50~60 DEG C, maintain pH value 5~6 with 200-
500r/min rotating speeds stir and drip performed polymer at a slow speed with 10~30ml/min, after 100~150min of arrest reaction, cooling
To 15~25 DEG C, is then adjusted pH value with sodium hydroxide and terminated to 8~9 and reacted；
The washing and drying be：
It adds urea and removes residual formaldehyde, washed with hot ethanol and hot water after suction filtration, then be dried in vacuo.
A kind of preparation method of temperature adjustment antimicrobial pearl regenerated celulose fibre of the present invention, melamine, formaldehyde are molten
The mass ratio of liquid and distilled water is 1: 1~2: 1~2；Wherein a concentration of 30~50wt% of formalin.
A kind of preparation method of temperature adjustment antimicrobial pearl regenerated celulose fibre of the present invention, paraffin, emulsifier and goes
The mass ratio of ionized water is 1: 0.5~2: 5~10；High speed emulsification times are 30~40min；The quality of pearl powder and dispersant
Than being 5~10: 1；The mass ratio of pearl powder and paraffin is 0.5~2: 1；The dispersant is propylene glycol block polyether；Paraffin
Mass ratio with performed polymer is 0.5~2: 1.
A kind of each method processed of temperature adjustment antimicrobial pearl regenerated celulose fibre of the present invention, the modulation additive
Mother liquor is：Under room temperature, by inorganic antibacterial particle, anion surfactant and distilled water with 0.02-0.04: 0.004-0.006:
1 quality adjusts pH value and is stood, waited for molten with the rotating speed cutting 20-40min of 2000-4000r/min to 9-10 than wiring solution-forming
After liquid is transparent, temperature control pearl microcapsules are added and stir evenly；The mass ratio of pearl microcapsules and inorganic antibacterial particle is 5-10: 1.
The present invention also proposes a kind of temperature adjustment antimicrobial pearl regenerated celulose fibre prepared by method made above, temperature adjustment
Antimicrobial pearl regenerated celulose fibre by regenerated celulose fibre, account for the temperature control pearl microcapsules of gross mass 5-15% and account for total matter
Measure the inorganic antibacterial particle composition of 0.5-1.5%；Answering of forming is blended by pearl powder with paraffin for the temperature control health care microcapsules
It closes core material and is made of the wall material that high molecular polymer is constituted；The mass ratio of the composite core material and wall material is 0.3~3:
1；Pearl powder average grain diameter≤1.2 μm, the pearl powder more than 2 μm of grain sizes are not more than 10%；The microcapsules
Average grain diameter≤3 μm, the microcapsules more than 5 μm of grain sizes are not more than 10%；The inorganic antibacterial particle is metal ion type
Antiseptic.
As preferred technical solution：
A kind of temperature adjustment antimicrobial pearl regenerated celulose fibre of the present invention, the high molecular polymer of the wall material is poly-
Urea, polyester resin, Lauxite, gelatin, poly- polyacid or melamine resin.
A kind of temperature adjustment antimicrobial pearl regenerated celulose fibre of the present invention, pearl powder in the composite core material with
The mass ratio of the paraffin is 0.5~2: 1.
A kind of temperature adjustment antimicrobial pearl regenerated celulose fibre of the present invention, the metal ion type antiseptic are silver
Ion, copper ion, zinc ion inorganic antiseptic, average grain diameter≤2 μm.
A kind of temperature adjustment antimicrobial pearl regenerated celulose fibre of the present invention, the regenerated celulose fibre is using wood
The regenerated cellulose staple fiber or long filament obtained by spinning solution spinning that one or more of slurry, bamboo pulp or cotton pulp are mixed with,
Including viscose glue, bamboo fibre, tencel or Modal.
Microcapsules technology is a kind of molecule to be overmolding to the new of core-wall shell structure particle using filmogen
Type technology.The formation basic theory of microcapsules makes high molecular polymer adsorption precipitation in molecule (solid, liquid or gas)
Periphery makes high molecular polymer form a film, forms shell then by changing the reaction condition of polymer.It is small in microcapsules
Particle is referred to as core material, and shell is referred to as wall material.The mass ratio of wall material/core material of microcapsules and turning for modulation molecule emulsion
Speed influences the clad ratio of microcapsules, the size of permeability and grain size.
Phase-change material refer under the variation of ambient temperature, structure mutually occur " solid-solid ", " solid-liquid ", " Gu-vapour " or
" liquid-vapour " changes and reversible material.In recent years, latent with absorbing or discharging big calorimetric in phase transition process due to phase-change material
The characteristic of energy, the material have been greatly developed in the application of heat accumulation engineering field.There are many phase-change material type, including paraffin
Class, crystalline hydrate salt, eutectic hydrated salt, polyethylene glycol, fatty acid and linear paraffin etc..Wherein paraffin is comprising straight chain alkane
The mixture of hydrocarbon, isoparaffin, cycloalkane has enthalpy change larger in phase transformation, good reversibility, temperature-controllable and at low cost etc.
Advantage；In addition, when adding high heat conduction particle in additive, the phase-change thermal storage performance of paraffin can be improved.
Adsorption combined is blended by pearl powder and paraffin in temperature control pearl microcapsules made from technical solution of the present invention, core material
It forms, under the action of auxiliary agent, the microcellular structure and configuration of surface of pearl powder can effectively receive or Adsorption Paraffin, microcapsules
Clad ratio, the size of permeability and grain size it is easily controllable；Temperature control pearl uniform microcapsule obtained is implanted into regenerated fiber
In cellulose fiber, pearl weaving can be made to take the influence of product not climate variation, can ensure that its due wearing comfort and strong
Change health-care efficacy.Its mechanism of action is as follows：When ambient temperature increases, the paraffin core material being embedded in pearl microcapsules will produce
" solid-liquid " phase transformation, in the process, paraffin heat absorption heat accumulation makes the reduction of web surface temperature, wearer that can experience pearl particles
The pleasantly cool sense discharged；When ambient temperature reduces, paraffin will produce " liquid-solid " phase transformation, and in the process, paraffin releases heat
Amount makes web surface temperature increase, even if in winter, wearer will not experience the excessively cool discomfort of underwear fabric；Together
When, due to intrastitial pearl powder temperature increase so that its in winter trace element release rate and far infrared normal direction
Emissivity is improved significantly, and strengthens the subcutaneous microcirculation of human body, improves absorption of the human body to pearl active ingredient.
Inorganic antibacterial particle is equably implanted into regenerated celulose fibre by technical solution of the present invention, can significantly increase pearl
The antibiotic property of product is taken in weaving；When the inorganic antibacterial particle has good thermal conductivity, the phase of temperature control microcapsules can be strengthened
Become heat storage function.
Core material can be made to avoid work in-process impaired under the package of wall material or dissolve with microcapsules technology, work(can be made
The incompatible core material ingredient of energy property, which is uniformly dispersed, to be blended in main material, and can control the rate of release of core material in the application.Silver
Based inorganic antibacterial agent has the characteristics that safe, has a broad antifungal spectrum, heat-resist, service life is long, it has also become inorganic in recent years
Anti-biotic material is studied and a big hot spot of application field.Therefore, the above temperature control antimicrobial pearl microcapsules technology is applied into pearl
In the production of regenerated celulose fibre, the deficiencies in the prior art can be efficiently solved.
Advantageous effect
Compared with prior art, temperature adjustment antimicrobial pearl microcapsules technology of the present invention has the beneficial effect that：
(1) tune for the textile that the temperature adjustment antimicrobial pearl regenerated celulose fibre of technical solution of the present invention processing gained makes
Temperature function can effectively keep taking the comfort temperature between product and human body；The far infrared method of winter pearl micro-particle when taking can be enhanced
To emissivity, micro- burst size is improved, skin-protection and health-care effect of product is enhanced.
(2) technical solution of the present invention can be such that pearl particles are uniformly and stably dispersed in spinning solution, eliminate pearl particles
Block spinneret orifice phenomenon, hence it is evident that improve production efficiency；Simultaneously avoid pearl powder precipitation and caused by valuable raw material damage
It loses, to be greatly lowered production cost；Inorganic antiseptic is uniformly and stably dispersed in regenerated cellulose, has both enhanced weaving
The antibacterial functions of product, and the phase-change thermal storage function of temperature control microcapsules can be strengthened.
(3) the temperature control pearl microcapsules not only high temperature resistant, but also acid and alkali-resistance prepared by technical solution of the present invention, is avoided that pearl
Grain directly contacts and causes the degradation of pearl particles with acid solution in spinning coagulation bath, it is ensured that the active ingredient of pearl powder.
(4) textile that the temperature adjustment antimicrobial pearl regenerated celulose fibre of technical solution of the present invention processing gained makes is anti-
Bacterium function can effectively inhibit the growth and breeding of bacterium and fungi under a home from home, it is ensured that the comfort of product reaches cleaning
Hygienic, cool in summer and warm in winter takes effect.
Specific implementation mode
The invention will be further elucidated with reference to specific embodiments.It should be understood that these embodiments are merely to illustrate this hair
It is bright rather than limit the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, art technology
Personnel can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Fixed range.
A kind of temperature adjustment antimicrobial pearl regenerated celulose fibre of the present invention, temperature adjustment antimicrobial pearl regenerated celulose fibre is by again
Raw cellulose fibre accounts for the temperature control pearl microcapsules of gross mass 5-15% and accounts for the inorganic antibacterial particle of gross mass 0.5-1.5%
Composition；The wall that the composite core material formed is blended with paraffin by pearl powder and is made of high molecular polymer for temperature control health care microcapsules
Material is formed；Composite core material and the mass ratio of wall material are 0.3~3: 1；Pearl powder average grain diameter≤1.2 μm are more than 2 μm of grain sizes
Pearl powder be not more than 10%；Average grain diameter≤3 μm of microcapsules, the microcapsules more than 5 μm of grain sizes are not more than 10%；It is inorganic
Antibacterial particle is metal ion type antiseptic.
Wherein, the high molecular polymer of the wall material is polyureas, polyester resin, Lauxite, gelatin, poly- polyacid or close
Polyimide resin.
Wherein, the mass ratio of the pearl powder in the composite core material and the paraffin is 0.5~2: 1.
Wherein, metal ion type antiseptic is silver ion, copper ion, zinc ion inorganic antiseptic, average grain diameter≤2 μm.
Wherein, the spinning solution that regenerated celulose fibre is mixed with using one or more of wood pulp, bamboo pulp or cotton pulp
Regenerated cellulose staple fiber obtained by spinning or long filament, including viscose glue, bamboo fibre, tencel or Modal.
Embodiment 1
A kind of preparation method of temperature adjustment antimicrobial pearl regenerated celulose fibre, step are：Prepare the micro- glue of temperature control pearl
--- modulation additive mother liquor --- prepares co-blended spinning liquid --- spinning --- post-processing to capsule.
First, temperature control pearl microcapsules are prepared, step is：Prepare performed polymer --- it is total with fire stons wax to prepare pearl powder
Mixed composite core material lotion --- polymerisation film forming --- is washed and drying；
Wherein, preparing performed polymer step is：
By the first of melamine, a concentration of 37wt% (37% is the common-use size of commercial product) that mass ratio is 1: 2: 2
Aldehyde solution and distilled water mixing adjust pH value with triethanolamine and are warming up to 70 DEG C to 9, with mixing slowly to transparent for 200r/min
Viscous liquid；Performed polymer total amount is based on the 140% of Quality of Paraffin Waxes；
Prepare pearl powder is with paraffin composite core material emulsion step：
At a temperature of 40 DEG C, by the 250g30# paraffin of fusing, the phenylethylene-maleic anhydride that 130g mass fractions are 18%
Copolymer sodium salt solution and the mixing of 2000ml deionized waters, 40min is emulsified with high speed 8000r/min；With oil bath heating to 95 DEG C
250g pearls powder (0.8 μm of average grain diameter) and 30g propylene glycol block polyethers are added afterwards, continues to emulsify with 400r/min rotating speeds
10min cools to the acetic acid for being 10% with mass fraction after 30 DEG C and adjusts ph value of emulsion to 5；
Polymerisation film formation step is：
Pearl powder and paraffin composite core material emulsion are warmed to 50 DEG C, pH value 5 is maintained, is stirred with 200r/min rotating speeds
It mixes and performed polymer 350g is dripped at a slow speed with 10ml/min, after arrest reaction 100min, cool to 15 DEG C, then use hydroxide
Sodium adjusts pH value and terminates reaction to 9；
It washs and dries and be：
With lemon acid for adjusting pH value to 7.2,10g urea is added, after stirring 5min with 120r/min rotating speeds, vacuum filtration is real
Apply separation of solid and liquid；40 DEG C of remaining organic matters of hot ethanol 50ml removals are added, with 50 in vacuum drying chamber after 40 DEG C of hot water washings
DEG C temperature dries 120min, that is, a kind of temperature control pearl health-care microcapsules are made.
Secondly, modulation additive mother liquor includes：Under room temperature, by average grain diameter be 2 μm silver ion inorganic antiseptic, it is cloudy from
Sub- surfactant and distilled water, than wiring solution-forming, adjust pH value to 9, with 2000r/min's with 0.02: 0.004: 1 quality
Rotating speed cutting 20min is stood, and after solution is transparent, the temperature control pearl microcapsules (mass ratio of microcapsules and silver ion particle is added
It is 10: 1) stirs evenly.
Then, preparing co-blended spinning liquid is：By additive mother liquor in 9% ratio of spinning viscose gross mass, spinning is injected
It is blended in stoste.
Finally, spinning is carried out with postprocessing working procedures by viscose staple fibre common process.
In gained temperature adjustment antimicrobial pearl viscose staple fibre, pearl powder content 4.8%；Silver-ion antibiotic agent content 0.8%；
Fiber thermoregulation temperature：18-29℃；When 5-10 DEG C of environment temperature, the far infrared normal emittance of pearl micro-particle improves 7-10%；It is fine
Dimension physical mechanical property meets GB/T 14463-2008；It is staphylococcus aureus, big by GB/T 20944 (textile) standard
The bacteriostasis rate of enterobacteria and Candida albicans is >=90%.
Embodiment 2
A kind of preparation method of temperature adjustment antimicrobial pearl regenerated celulose fibre, step are：Prepare the micro- glue of temperature control pearl
--- modulation additive mother liquor --- prepares co-blended spinning liquid --- spinning --- post-processing to capsule.
First, temperature control pearl microcapsules are prepared, step is：Prepare performed polymer --- it is total with fire stons wax to prepare pearl powder
Mixed composite core material lotion --- polymerisation film forming --- is washed and drying；
Wherein, preparing performed polymer step is：
By mass ratio be 1: 1.8: 2 melamine, the formalin of a concentration of 37wt% and distilled water mix, with three second
Hydramine adjusts pH value to 9,68 DEG C is warming up to, with mixing slowly to clear viscous shape liquid for 300r/min；Performed polymer total amount is pressed
160% meter of Quality of Paraffin Waxes；
Prepare pearl powder is with paraffin composite core material emulsion step：
At a temperature of 50 DEG C, by the 250g30# paraffin of fusing, the phenylethylene-maleic anhydride that 130g mass fractions are 18%
After copolymer sodium salt solution and the mixing of 1800ml deionized waters, 30min is emulsified with high speed 9000r/min；Then oil bath heating is used
To 98 DEG C, 300g pearls powder (1 μm of average grain diameter) and 35g dispersant propylene glycol block polyethers is added, continues with 600r/min
After rotating speed emulsifies 15min, 35 DEG C are cooled to, with lemon acid for adjusting pH value to 5.5；
Polymerisation film formation step is：
Pearl powder and paraffin composite core material emulsion are warmed to 60 DEG C, pH value 5.5 is maintained, with 250r/min rotating speeds
Stir and with dropwise addition at a slow speed the performed polymer 400g, arrest reaction 150min of 15ml/min after, cool to 25 DEG C, then use hydroxide
Sodium adjusts pH value and terminates reaction to 9；
It washs and dries and be：
With lemon acid for adjusting pH value to 7.0,12g urea is added, after stirring 8min with 100r/min rotating speeds, vacuum filtration is real
Apply separation of solid and liquid；42 DEG C of remaining organic matters of hot ethanol 40ml removals are added, with 55 in vacuum drying chamber after 42 DEG C of hot water washings
DEG C temperature dries 100min, that is, a kind of temperature control pearl health-care microcapsules are made.
Secondly, modulation additive mother liquor includes：Under room temperature, by average grain diameter be 1.6 μm of copper ion inorganic antiseptics, it is cloudy from
Sub- surfactant and distilled water, than wiring solution-forming, adjust pH value to 10, with 4000r/min's with 0.04: 0.006: 1 quality
Rotating speed cutting 40min is stood, and after solution is transparent, the temperature control pearl microcapsules (mass ratio of microcapsules and copper ion particle is added
It is 9: 1) stirs evenly.
Then, preparing co-blended spinning liquid is：By additive mother liquor in 10% ratio of spinning viscose gross mass, spinning is injected
It is blended in stoste.
Finally, spinning is carried out with postprocessing working procedures by viscose staple fibre common process.
In gained temperature adjustment antimicrobial pearl viscose staple fibre, pearl powder content 5.1%；Copper ion antimicrobial levels 1.2%；
Fiber thermoregulation temperature：18-28℃；When 5-10 DEG C of environment temperature, the far infrared normal emittance of pearl micro-particle improves 8-10%；It is fine
Dimension physical mechanical property meets GB/T 14463-2008；It is staphylococcus aureus, big by GB/T 20944 (textile) standard
The bacteriostasis rate of enterobacteria and Candida albicans is >=90%.
Embodiment 3
A kind of preparation method of temperature adjustment antimicrobial pearl regenerated celulose fibre, step are：Prepare the micro- glue of temperature control pearl
--- modulation additive mother liquor --- prepares co-blended spinning liquid --- spinning --- post-processing to capsule.
First, temperature control pearl microcapsules are prepared, step is：Prepare performed polymer --- it is total with fire stons wax to prepare pearl powder
Mixed composite core material lotion --- polymerisation film forming --- is washed and drying；
Wherein, preparing performed polymer step is：
By mass ratio be 1: 1.6: 1.8 melamine, the formalin of a concentration of 37wt% and distilled water mix, with three
Ethanol amine adjusts pH value to 8.5,70 DEG C is warming up to, with mixing slowly to clear viscous shape liquid for 250r/min；Performed polymer is total
Amount is based on the 150% of Quality of Paraffin Waxes；
Prepare pearl powder is with paraffin composite core material emulsion step：
At a temperature of 45 DEG C, by the 280g paraffin of fusing, the styrene-maleic anhydride copolymer that 140g mass fractions are 18%
After object sodium salt solution and the mixing of 2000ml deionized waters, 30min is emulsified with high speed 8000r/min；Then with oil bath heating to 92
DEG C, 300g pearls powder (1 μm of average grain diameter) and 30g dispersant propylene glycol block polyethers is added, continues with 400r/min rotating speeds
After emulsifying 15min, 30 DEG C are cooled to, with lemon acid for adjusting pH value to 5；
Polymerisation film formation step is：
Pearl powder and paraffin composite core material emulsion are warmed to 58 DEG C, pH value 5 is maintained, is stirred with 220r/min rotating speeds
Mix, and with dropwise addition at a slow speed the performed polymer 420g, arrest reaction 100min of 18ml/min after, cool to 20 DEG C, then use hydroxide
Sodium adjusts pH value and terminates reaction to 9；
It washs and dries and be：
With lemon acid for adjusting pH value to 7.3,12g urea is added, after stirring 5min with 120r/min rotating speeds, vacuum filtration is real
Apply separation of solid and liquid；40 DEG C of remaining organic matters of hot ethanol 50ml removals are added, with 60 in vacuum drying chamber after 45 DEG C of hot water washings
DEG C temperature dries 120min, that is, a kind of temperature control pearl health-care microcapsules are made.
Secondly, modulation additive mother liquor includes：Under room temperature, by average grain diameter be 1.8 μm of zinc ion inorganic antiseptics, it is cloudy from
Sub- surfactant and distilled water, than wiring solution-forming, adjust pH value to 9, with 2500r/min's with 0.03: 0.005: 1 quality
Rotating speed cutting 25min is stood, and after solution is transparent, the temperature control pearl microcapsules (mass ratio of microcapsules and zinc ion particle is added
It is 8: 1) stirs evenly.
Then, preparing co-blended spinning liquid is：By additive mother liquor in 8% ratio of spinning viscose gross mass, spinning is injected
It is blended in stoste.
Finally, spinning is carried out with postprocessing working procedures by viscose filament yarn common process.
In gained temperature adjustment antimicrobial pearl viscose filament yarn, pearl powder content 4.8%；Zinc ion antimicrobial levels 1.1%；It is fine
Tie up temperature adjustment temperature：18-29℃；When 5-10 DEG C of environment temperature, the far infrared normal emittance of pearl micro-particle improves 8-10%；Fiber
Physical mechanical property meets GB/T 13758-2008；By GB/T 20944 (textile) standard, staphylococcus aureus, large intestine
The bacteriostasis rate of bacillus and Candida albicans is >=90%.
Embodiment 4
A kind of preparation method of temperature adjustment antimicrobial pearl regenerated celulose fibre, step are：Prepare the micro- glue of temperature control pearl
--- modulation additive mother liquor --- prepares co-blended spinning liquid --- spinning --- post-processing to capsule.
First, temperature control pearl microcapsules are prepared, step is：Prepare performed polymer --- it prepares pearl powder and is blended with paraffin
Composite core material lotion --- polymerisation film forming --- is washed and drying；
Wherein, preparing performed polymer step is：
By mass ratio be 1: 1.6: 2 melamine, the formalin of a concentration of 40wt% and distilled water mix, with three second
Hydramine adjusts pH value to 8,72 DEG C is warming up to, with mixing slowly to clear viscous shape liquid for 350r/min；Performed polymer total amount is pressed
150% meter of Quality of Paraffin Waxes；
Prepare pearl powder is with paraffin composite core material emulsion step：
At a temperature of 45 DEG C, by the 250g30# paraffin of fusing, the phenylethylene-maleic anhydride that 130g mass fractions are 18%
After copolymer sodium salt solution and the mixing of 1800ml deionized waters, 35min is emulsified with high speed 7000r/min；Then oil bath heating is used
To 90 DEG C, 300g pearls powder (1 μm of average grain diameter) and 30g dispersant propylene glycol block polyethers is added, continues with 500r/min
After rotating speed emulsifies 12min, 30 DEG C are cooled to, with lemon acid for adjusting pH value to 5；
Polymerisation film formation step is：
Pearl powder and paraffin composite core material emulsion are warmed to 55 DEG C, pH value 5 is maintained, is stirred with 250r/min rotating speeds
Mix, and with dropwise addition at a slow speed the performed polymer 375g, arrest reaction 120min of 18ml/min after, cool to 25 DEG C, then use hydroxide
Sodium adjusts pH value and terminates reaction to 8.5；
It washs and dries and be：
With lemon acid for adjusting pH value to 7.0,10g urea is added, after stirring 6min with 110r/min rotating speeds, vacuum filtration is real
Apply separation of solid and liquid；42 DEG C of remaining organic matters of hot ethanol 45ml removals are added, with 55 in vacuum drying chamber after 45 DEG C of hot water washings
DEG C temperature dries 110min, that is, a kind of temperature control pearl health-care microcapsules are made.
Secondly, modulation additive mother liquor includes：Under room temperature, by average grain diameter be 1.5 μm of copper ion inorganic antiseptics, it is cloudy from
Sub- surfactant and distilled water, than wiring solution-forming, adjust pH value to 10, with 3000r/min's with 0.04: 0.004: 1 quality
Rotating speed cutting 30min is stood, and after solution is transparent, the temperature control pearl microcapsules (mass ratio of microcapsules and copper ion particle is added
It is 8: 1) stirs evenly.
Then, preparing co-blended spinning liquid is：By additive mother liquor in 8.5% ratio of spinning viscose gross mass, injection is spun
It is blended in silk stock solution.
Finally, spinning is carried out with postprocessing working procedures by viscose staple fibre common process.
In gained temperature adjustment antimicrobial pearl viscose staple fibre, pearl powder content 4.9%；Copper ion antimicrobial levels 1.2%；
Fiber thermoregulation temperature：17-29℃；When 5-10 DEG C of environment temperature, the far infrared normal emittance of pearl micro-particle improves 7-9%；It is fine
Dimension physical mechanical property meets GB/T 14463-2008；It is staphylococcus aureus, big by GB/T 20944 (textile) standard
The bacteriostasis rate of enterobacteria and Candida albicans is >=90%.
Embodiment 5
A kind of preparation method of temperature adjustment antimicrobial pearl regenerated celulose fibre, step are：Prepare the micro- glue of temperature control pearl
--- modulation additive mother liquor --- prepares co-blended spinning liquid --- spinning --- post-processing to capsule.
First, temperature control pearl microcapsules are prepared, step is：Prepare performed polymer --- prepare pearl powder, oxide powder and zinc
Body is washed with paraffin composite core material emulsion --- polymerisation film forming --- and drying；
Wherein, preparing performed polymer step is：
By mass ratio be 1: 2: 1.8 melamine, the formalin of a concentration of 37wt% and distilled water mix, with three second
Hydramine adjusts pH value to 9,65 DEG C is warming up to, with mixing slowly to clear viscous shape liquid for 200r/min；Performed polymer total amount is pressed
140% meter of Quality of Paraffin Waxes；
Preparing pearl powder, Zinc oxide powder and paraffin composite core material emulsion step is：
At a temperature of 40 DEG C, by 250g paraffin, the styrene-maleic anhydride copolymer sodium salt that 130g mass fractions are 18%
Solution and the mixing of 2000ml deionized waters, 40min is emulsified with high speed 8000r/min；With oil bath heating to 200g is added after 95 DEG C
Pearl powder (0.8 μm of average grain diameter), 50g Zinc oxide powders (1 μm of average grain diameter) and 30g propylene glycol block polyethers, continue with
500r/min rotating speeds emulsify 10min, cool to the acetic acid for being 10% with mass fraction after 30 DEG C and adjust ph value of emulsion to 5；
Polymerisation film formation step is：
Pearl powder, Zinc oxide powder and paraffin composite core material emulsion are warmed to 50 DEG C, maintain pH value 5, with
200r/min rotating speeds stir and with dropwise addition at a slow speed the performed polymer 350g, arrest reaction 150min of 10ml/min after, cool to 15 DEG C,
Then it is adjusted pH value with sodium hydroxide and is terminated to 9 and reacted；
It washs and dries and be：
With lemon acid for adjusting pH value to 7.2,12g urea is added, after stirring 7min with 100r/min rotating speeds, vacuum filtration is real
Apply separation of solid and liquid；45 DEG C of remaining organic matters of hot ethanol 50ml removals are added, with 60 in vacuum drying chamber after 40 DEG C of hot water washings
DEG C temperature dries 110min, that is, a kind of temperature control pearl health-care microcapsules are made.
Secondly, modulation additive mother liquor includes：Under room temperature, by average grain diameter be 1 μm copper ion inorganic antiseptic, it is cloudy from
Sub- surfactant and distilled water, than wiring solution-forming, adjust pH value to 10, with 2800r/min's with 0.03: 0.004: 1 quality
Rotating speed cutting 40min is stood, and after solution is transparent, the temperature control pearl microcapsules (mass ratio of microcapsules and copper ion particle is added
It is 10: 1) stirs evenly.
Then, preparing co-blended spinning liquid is：By additive mother liquor in 9.5% ratio of spinning viscose gross mass, injection is spun
It is blended in silk stock solution.
Finally, spinning is carried out with postprocessing working procedures by viscose filament yarn common process.
In gained temperature adjustment antimicrobial pearl viscose filament yarn, pearl powder content 4.2%；Zinc oxide antimicrobial levels 1.0%；Oxygen
Change copper antimicrobial levels 0.7%；Fiber thermoregulation temperature：19-28℃；When 5-10 DEG C of environment temperature, the far infrared method of pearl micro-particle
7-9% is improved to emissivity；Fibrous physics mechanical performance meets GB/T 13758-2008；It is marked by GB/T 20944 (textile)
Standard, the bacteriostasis rate of staphylococcus aureus, Escherichia coli and Candida albicans is >=90%.
Claims (6)
1. a kind of preparation method of temperature adjustment antimicrobial pearl regenerated celulose fibre, which is characterized in that step is：Prepare temperature control pearl
--- modulation additive mother liquor --- prepares co-blended spinning liquid --- spinning --- post-processing, obtains temperature adjustment antimicrobial pearl again microcapsules
Raw cellulose fibre；Average grain diameter≤3 μm of the microcapsules, the microcapsules more than 5 μm of grain sizes are not more than 10%；
The step of preparation temperature control pearl microcapsules is：Prepare performed polymer --- prepare pearl powder and paraffin composite core
Material lotion --- polymerisation film forming --- is washed and drying；
The performed polymer step for preparing is：
Melamine, formalin and distilled water are mixed, pH value is adjusted to 8~9,60~80 DEG C is warming up to, with 200-500r/
Min is mixed slowly to clear viscous shape liquid；The mass ratio of melamine, formalin and distilled water is 1: 1~2: 1~2；Its
A concentration of 30~50wt% of middle formalin；
The preparation pearl powder is with paraffin composite core material emulsion step：
At a temperature of 40-50 DEG C, with high speed 6000-10000r/min after the paraffin, emulsifier and deionized water of fusing are mixed
Pearl powder and dispersant is added then with oil bath heating to 90-99 DEG C in emulsification, continues to emulsify with 400-600r/min rotating speeds
After 10~15min, 30-40 DEG C is cooled to, with weak acid for adjusting pH value to 5~6；
The mass ratio of paraffin, emulsifier and deionized water is 1: 0.5~2: 5~10；High speed emulsification times are 30~40min；It is precious
The mass ratio of pearl powder and dispersant is 5~10: 1；The mass ratio of pearl powder and paraffin is 0.5~2: 1；The dispersant is
Propylene glycol block polyether；The mass ratio of paraffin and performed polymer is 0.5~2: 1；
The polymerisation film formation step is：
Pearl powder and paraffin composite core material emulsion are warmed to 50~60 DEG C, maintain pH value 5~6 with 200-500r/min
Rotating speed stirs and drips performed polymer at a slow speed with 10~30ml/min, after 100~150min of arrest reaction, cools to 15~25
DEG C, it is then adjusted pH value with sodium hydroxide and is terminated to 8~9 and reacted；
The washing and drying be：
It adds urea and removes residual formaldehyde, washed with hot ethanol and hot water after suction filtration, then be dried in vacuo.
2. a kind of preparation method of temperature adjustment antimicrobial pearl regenerated celulose fibre according to claim 1, which is characterized in that
The modulation additive mother liquor is：Under room temperature, by inorganic antibacterial particle, anion surfactant and distilled water with 0.02~
0.04: 0.004~0.006: 1 quality is adjusted pH value to 9~10, is cut with the rotating speed of 2000-4000r/min than wiring solution-forming
20~40min is cut, is stood, after solution is transparent, temperature control pearl microcapsules is added and stir evenly；Pearl microcapsules and inorganic antibacterial
The mass ratio of particle is 5~10: 1.
3. using a kind of made from a kind of preparation method of temperature adjustment antimicrobial pearl regenerated celulose fibre as described in claim 1
Temperature adjustment antimicrobial pearl regenerated celulose fibre, it is characterized in that：Temperature adjustment antimicrobial pearl regenerated celulose fibre is by regenerated cellulose fibre
It ties up, account for the temperature control pearl microcapsules of gross mass 5~15% and account for the inorganic antibacterial particle composition of gross mass 0.5~1.5%；It is described
The wall material institute that the composite core material formed is blended with paraffin by pearl powder and is made of high molecular polymer for temperature control health care microcapsules
Composition；The mass ratio of the composite core material and wall material is 0.3~3: 1；Pearl powder average grain diameter≤1.2 μm, greatly
It is not more than 10% in the pearl powder of 2 μm of grain sizes；The inorganic antibacterial particle is metal ion type antiseptic.
4. a kind of temperature adjustment antimicrobial pearl regenerated celulose fibre according to claim 3, which is characterized in that the composite core
The mass ratio of pearl powder and the paraffin in material is 0.5~2: 1.
5. a kind of temperature adjustment antimicrobial pearl regenerated celulose fibre according to claim 3, which is characterized in that the metal
Ionic antiseptic is silver ion, copper ion, zinc ion inorganic antiseptic, average grain diameter≤2 μm.
6. a kind of temperature adjustment antimicrobial pearl regenerated celulose fibre according to claim 3, which is characterized in that the regeneration
Cellulose fibre is that the regeneration obtained by the spinning solution spinning that is mixed with using one or more of wood pulp, bamboo pulp or cotton pulp is fine
The plain staple fiber of dimension or long filament, specially viscose glue, bamboo fibre, tencel or Modal.
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