CN106192054A - Environment-friendly type regeneration negative ion far-infrared function flame retardant polyester staple fibre - Google Patents
Environment-friendly type regeneration negative ion far-infrared function flame retardant polyester staple fibre Download PDFInfo
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- CN106192054A CN106192054A CN201610578725.8A CN201610578725A CN106192054A CN 106192054 A CN106192054 A CN 106192054A CN 201610578725 A CN201610578725 A CN 201610578725A CN 106192054 A CN106192054 A CN 106192054A
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- infrared
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/78—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products
- D01F6/84—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products from copolyesters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Artificial Filaments (AREA)
Abstract
A kind of environment-friendly type regeneration negative ion far-infrared function flame retardant polyester staple fibre, comprises the steps: S1: the preparation of far-infrared powder liquid solution: S2: fire retardant is the most pre-: S3: regenerate the synthesis of far infrared fire retardant polyester resin.The slice spinning forming of the preparation of the present invention, far IR fibre is best in quality;The conjugation of storeroom can be greatly enhanced, be effectively improved far IR fibre mechanical property, improve fibre strength by a relatively large margin.Select suitable difunctional halogen-free flame retardants, first fire retardant is carried out special pre-treatment, fire retardant free flame retardant agent content in polycondensation phase participates in copolyreaction, and end product can be made the lowest, it is ensured that the performance of negative ion far-infrared flame retardant polyester.
Description
Technical field
The invention belongs to fibrous material field, particularly to the environment-friendly type regeneration negative ion far-infrared short fibre of function flame-resistant terylene
Dimension.
Background technology
Ordinary polyester fiber has excellent wearability and the scope of application widely, has exceeded cotton as textile raw material consumption
Flower, but also exists some serious shortcomings, on the one hand the warmth retention property of dacron is poor and the goods such as plastics, chemical fibre discarded after not
Degrade easily, thus directly utilize fossil resource production in enormous quantities polyster fibre and resulted in the great wasting of resources and environment dirt
Dye;On the other hand, the limited oxygen index (LOI) of terylene is about 21, along with the extensive application of fabric, and its fire potential
Danger also becomes increasingly conspicuous.The health-care effect of human body is confirmed by negative aeroion already by medical circle, the most increasingly by vast consumption
Person is cognitive, and Negative ionic textile can constantly release negative aeroion, to reach health care and to eliminate abnormal flavour, purify the dual of air
Effect.Negative ionic textile owing to directly wearing, large area and contact human skin, the heat energy of available human body and human body
Accelerate the generation of negative aeroion with rubbing of skin during motion, i.e. form an anion air layer at skin with check room,
Be conducive to oxygen-derived free radicals Non-toxic in human body, eliminate the oxygen-derived free radicals multiple harm to health.The biological effect of far infrared
Its frequency should be with to constitute the molecule of biological cell, intraatomic vibration ratio identical, so easily being absorbed by organism
Making intramolecular vibration strengthen, activation histiocyte blood circulation promoting accelerates metabolism.Due to the effect of far infrared, make
Molecular entergy level in organism is excited and is in higher vibration level, and this will improve the biomacromolecules such as nucleic acid protein
Activity, thus play it and adjust organism metabolism, improve the effect of immunity of organisms.By anion function, far-infrared functional, fire-retardant
It is the starting point of the present invention that function, environment-friendly function combine.
Anion can improve atmosphere quality, protection health, is the important of measurement air quality clean-up performance
One of index.In recent years, dense population areas, big city also exists anion and consumes abnormal serious protrusion phenomenon, and this allows for newly
The research and development of type anion releasable material become the focus in Research of Environmental Sciences field.Far infrared shakes with human inner cell's molecule
Dynamic frequency is close, " life light wave " penetrate into internal after, the atom of human body cell and the resonance of molecule will be caused, through sympathetic response
Absorbing, between molecule, frictional heat forms thermal response, promotes subcutaneous deep temperature to rise, and makes Marjoram Extract, accelerates blood
Circulation, is conducive to removing blood vessel and hoards thing and internal harmful substance, will harm metabolic obstacle cleaning, again make tissue multiple
Live, promote that ferment generates, reach to activate histiocyte, prevent aging, the purpose of strengthening immune system.So far infrared for
The multiple disease that blood circulation and microcirculation disturbance cause is respectively provided with improvement and preventive and therapeutic effect.Far infrared is applied to anion
Terylene short fiber is also made vehicle material, household material, heat insulating material formed etc. can effectively be improved living environment, improves health.
But terylene is a kind of inflammable substance, it is widely used and adds the probability that fire occurs, and this is to the person and property safety band
Carry out hidden danger.Therefore, coordinating flame-retarded technology, the application of terylene short fiber will be more wide.
The far-infrared negative-ion chopped fiber provided in the market mainly uses Surface-micromachining process fine to conventional polyester
Dimension carries out arrangement and prepares, or adds far-infrared negative-ion master batch making fiber in primary polyester slice, though the former can temporarily protect
Hold far-infrared negative-ion function, but the time one is long or can lose effect after washing, and the latter's far-infrared negative-ion function effect
Fruit is preferable, and function is lasting, but owing to manufacturing cost is higher, have impact on promoting the use of of product.
In the prior art, oneself has many foreign literatures fine to health fiber or far IR fibre or their mixed function
Dimension and fabric thereof have carried out deep discussion and discussion, and also oneself comes into the market to possess the fiber of this respect function and fabric.But
These functional fibres or there is far-infrared functional, or there is negative ion-releasing function, act on the most single.
Summary of the invention
It is an object of the invention to as overcoming above-mentioned the deficiencies in the prior art, it is provided that a kind of environment-friendly type regeneration negative ion far-infrared
Function flame retardant polyester staple fibre, with the multifunctionality of further abundant fiber, the present invention by negative ion far-infrared additive with spy
Different technique is added in flame retardant polyester section, produces far flame retardant polyester staple fibre capable of releasing negative ion, the present invention
Product have forever discharge hydroxyl group anion (H3O2-), radiation wavelength is up to the function of far infrared of 4 μm-18 μm, limit oxygen
Index is up to 36.8%.
For achieving the above object, the present invention uses following technical proposals:
A kind of environment-friendly type regeneration negative ion far-infrared function flame retardant polyester staple fibre, comprises the steps:
S1: the preparation of far-infrared powder liquid solution: use the modification that sand milling is combined with surfactant;
S2: fire retardant is the most pre-: process fire retardant after special pre-treatment;
S3: regeneration far infrared fire retardant polyester resin synthesis: by the p-phthalic acid after polyester bottle slice alcoholysis, ethylene glycol,
Catalyst by proportion puts in esterifying kettle after making beating, and glycolysis temperature controls Stress control between 245-260 DEG C, in still and exists
0.1-0.3MPa, after PET powder degradation is complete, adds negative ion far-infrared powder body solution, fire retardant treatment fluid, polycondensation catalysis
Agent, imports after being warming up to 260 DEG C in polycondensation vessel, and condensation temperature controls as 275-285 DEG C, vacuum < 50Pa, mechanical agitation 1h-
After 96h stop stirring, cooled, pelletizing and be dried, prepare regeneration far infrared flame retardant polyester master batch;Described catalyst is acetic acid
Zinc;Described polycondensation catalyst is a kind of in TiO2/SiO2 colloidal sol, antimony glycol;Described fire retardant treatment fluid is decabrominated dipheny second
One in alkane, deca-BDE, triphenyl phosphate, triphenyl phosphate;;
S4: polyester master particle is dried process, and makes Direct-spinning of PET Fiber section;
S5: Direct-spinning of PET Fiber section is carried out melt spinning, and through winding, drawing-off, crimp, cool down after cut-out, pack into
Storehouse.
In described step S3, p-phthalic acid, ethylene glycol, the volume mass ratio of catalyst are: 5-20ml:2-8ml:1-8g.
Addition negative ion far-infrared powder body, fire retardant treatment fluid, polycondensation catalyst and the matter of auxiliary agent in described step S3
Amount volume ratio is 2-10g:0.5-1.5ml:0.08-0.3g:0.012-0.05g
In described step S1, negative ion far-infrared powder body is made up of the raw material of following weight portion: Fe2O33.0-10 part,SiO2
27.5-50 part, Al2O324-48 part, TiO230-90 part, B2O315.2-42 part, MgO 1-5 part, ZrO2 0.5-1.2 part,
ZnO 0.1-2 part, NiO 0.05-0.8 part, CuO 0.5-2.5 part.
Described step S4 is dried as condition as follows: first with the temperature drying 3 of 70~80 DEG C~4 hours, then heat up
To 100 DEG C of dryings 1~2 hours, then it is warming up to 120 DEG C of blended dryings 1~2 hours, finally be warming up to 145 DEG C of blended dryings
8 hours and more than, criteria thus the drying time be not less than 16 hours.
In described step S5, the technological parameter of drawing-off is as follows: drafting multiple: 3.4 times;Drawing temperature: profit bathes 65 DEG C;Steam
Vapour 100 DEG C;Crispation number: 8-9/25mm;Heat setting temperature: 120 DEG C.
The performance of the polyester staple fiber of preparation, far emissivity is 0.88, and radiation wavelength 4 μm-18 μm, anion is sent out
Raw amount reaches 3170/cm3, and fabric limited oxygen index reaches 36.8%.
Beneficial effects of the present invention:
1, the slice spinning forming of the preparation of the present invention, far IR fibre is best in quality;Storeroom can be greatly enhanced
Conjugation, is effectively improved far IR fibre mechanical property, improves fibre strength by a relatively large margin.Select suitable difunctional Halogen
Fire retardant, first carries out special pre-treatment by fire retardant, can make fire retardant in polycondensation phase participates in copolyreaction, and end product
Free flame retardant agent content is the lowest, it is ensured that the performance of negative ion far-infrared flame retardant polyester.
2, the present invention uses the difunctional halogen-free flame retardants of modification to participate in p-phthalic acid, ethylene glycol in polycondensation phase
Copolyreaction obtains fire-retardant slice, prepares permanent fire retardant terylene short fiber by melt spinning.Preparing environment-friendly type regeneration anion
Solving following technical barrier in far-infrared functional flame retardant polyester slicing processes, one is to prevent negative ion far-infrared powder body at ethylene glycol
Reuniting in solution and separate out, two is the spinnability improving environment-friendly type regeneration negative ion far-infrared function flame retardant polyester, and three is to realize
Polyester Halogen copolymerization is fire-retardant;Significant technology issues to be overcome in the preparation process of short fibre, i.e. by controlling in short fine production
Temperature during extrusion and pressure, maintain a difficult problem for the functional of fiber and intensity effectively.
3, the performance of polyester staple fiber prepared by the present invention, far emissivity is 0.88, radiation wavelength 4 μm-18 μm,
Anion-generating capacity reaches 3170/cm3, and fabric limited oxygen index reaches 36.8%.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 1 composite granule.
Fig. 2 is the scanning electron microscope comparison diagram of the fiber product of the embodiment of the present invention 1 preparation.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further elaborated, it should explanation, the description below merely to
Explain the present invention, its content is not defined.
Testing graininess use Qulter LS230 laser particle analyzer test, and combine employing SEM method carry out particle size distribution
Observe with granule-morphology.For the test of main function index, concrete method has, the method for testing of anion superfine powder
All use static testing, INSTRUMENT MODEL EB-12A ion tester;The method of testing of weaving finished product mainly uses dynamically survey
Examination method, INSTRUMENT MODEL is ITC-101 ion tester.The test of far infrared all band normal emittance index is measured section by China
Learn academy and country is infrared and industrial electroheat product quality supervision and inspection center uses and standard blackbody normal direction total radiation brightness
Comparative approach is measured.Limited oxygen index is tested by inspection center of Chinese textile industry community with flame spread rate.
Embodiment 1
A kind of environment-friendly type regeneration negative ion far-infrared function flame retardant polyester staple fibre, comprises the steps:
S1: the preparation of far-infrared powder liquid solution: use the modification that sand milling is combined with surfactant;
S2: fire retardant is the most pre-: process fire retardant after special pre-treatment;
S3: regeneration far infrared fire retardant polyester resin synthesis: by the p-phthalic acid after polyester bottle slice alcoholysis, ethylene glycol,
Catalyst by proportion puts in esterifying kettle after making beating, and glycolysis temperature controls between 245 DEG C, in still, Stress control exists
0.1MPa, after PET powder degradation is complete, adds negative ion far-infrared powder body solution, fire retardant treatment fluid, polycondensation catalyst,
Importing after being warming up to 260 DEG C in polycondensation vessel, it is 275 DEG C that condensation temperature controls, vacuum 50Pa, stops stirring after mechanical agitation 1h,
Cooled, pelletizing and being dried, prepares regeneration far infrared flame retardant polyester master batch;Described catalyst is zinc acetate;Described polycondensation is catalyzed
Agent is TiO2/SiO2 colloidal sol;Described fire retardant treatment fluid is TDE;
S4: polyester master particle is dried process, and makes Direct-spinning of PET Fiber section;
S5: Direct-spinning of PET Fiber section is carried out melt spinning, and through winding, drawing-off, crimp, cool down after cut-out, pack into
Storehouse.
In described step S3, p-phthalic acid, ethylene glycol, the volume mass ratio of catalyst are: 5ml:2ml:1g.
Addition negative ion far-infrared powder body, fire retardant treatment fluid, polycondensation catalyst and the matter of auxiliary agent in described step S3
Amount volume ratio is 2g:0.5ml:0.08g:0.012g
Described step S1 mid and far infrared powder body is made up of the raw material of following weight portion: Fe2O310 part, SiO2 50 parts,
Al2O348 part, TiO2 90 parts, B2O3 42 parts, MgO5 part, ZrO2 1.2 parts, ZnO 2 parts, NiO0.8 part, CuO2.5 part.
Described step S4 is dried as condition as follows: first with the temperature drying 4 hours of 70~80 DEG C, then heat to
100 DEG C of dryings 2 hours, then it is warming up to 120 DEG C of blended dryings 2 hours, finally it is warming up to 145 DEG C of blended dryings 8 hours
More than and, criteria thus the drying time is not less than 16 hours.
In described step S5, the technological parameter of drawing-off is as follows: drafting multiple: 3.4 times;Drawing temperature: profit bathes 65 DEG C;Steam
Vapour 100 DEG C;Crispation number: 9/25mm;Heat setting temperature: 120 DEG C.
The performance of the polyester staple fiber of preparation, far emissivity is 0.88, and radiation wavelength 4 μm-18 μm, anion is sent out
Raw amount reaches 3170/cm3, fabric limited oxygen index reaches 36.8%.
Embodiment 2
A kind of environment-friendly type regeneration negative ion far-infrared function flame retardant polyester staple fibre, comprises the steps:
S1: the preparation of far-infrared powder liquid solution: use the modification that sand milling is combined with surfactant;
S2: fire retardant is the most pre-: process fire retardant after special pre-treatment;
S3: regeneration far infrared fire retardant polyester resin synthesis: by the p-phthalic acid after polyester bottle slice alcoholysis, ethylene glycol,
Catalyst by proportion puts in esterifying kettle after making beating, and glycolysis temperature controls between 260 DEG C, in still Stress control at 0.1-
0.3MPa, after PET powder degradation is complete, adds negative ion far-infrared powder body solution, fire retardant treatment fluid, polycondensation catalyst,
Importing after being warming up to 260 DEG C in polycondensation vessel, it is 285 DEG C that condensation temperature controls, vacuum 30Pa, stops stirring after mechanical agitation 96h,
Cooled, pelletizing and being dried, prepares regeneration far infrared flame retardant polyester master batch;Described catalyst is zinc acetate;Described polycondensation is catalyzed
Agent is antimony glycol;Described fire retardant treatment fluid is deca-BDE;
S4: polyester master particle is dried process, and makes Direct-spinning of PET Fiber section;
S5: Direct-spinning of PET Fiber section is carried out melt spinning, and through winding, drawing-off, crimp, cool down after cut-out, pack into
Storehouse.
In described step S3, p-phthalic acid, ethylene glycol, the volume mass ratio of catalyst are: 20ml:8ml:8g.
Addition negative ion far-infrared powder body, fire retardant treatment fluid, polycondensation catalyst and the matter of auxiliary agent in described step S3
Amount volume ratio is 10g:1.5ml:0.3g:0.05g
Described step S1 mid and far infrared powder body is made up of the raw material of following weight portion: Fe2O33.0 parts, SiO227.5 part,
Al2O324 parts, TiO230 parts, B2O315.2 parts, MgO1 part, ZrO20.5 part, ZnO 0.1 part, NiO 0.05 part, CuO 0.5
Part.
Described step S4 is dried as condition as follows: first with the temperature drying 3 hours of 70 DEG C, then heat to 100 DEG C
Drying 1 hour, then be warming up to 120 DEG C of blended dryings hour, be finally warming up to 145 DEG C of blended dryings 8 hours and more than,
Criteria thus the drying time is not less than 16 hours.
In described step S5, the technological parameter of drawing-off is as follows: drafting multiple: 3.4 times;Drawing temperature: profit bathes 65 DEG C;Steam
Vapour 100 DEG C;Crispation number: 8/25mm;Heat setting temperature: 120 DEG C.
The performance of the polyester staple fiber of preparation, far emissivity is 0.88, radiation wavelength 4 μm μm, and anion occurs
Amount reaches 3170/cm3, fabric limited oxygen index reaches 36.8%.
Embodiment 3
A kind of environment-friendly type regeneration negative ion far-infrared function flame retardant polyester staple fibre, comprises the steps:
S1: the preparation of far-infrared powder liquid solution: use the modification that sand milling is combined with surfactant;
S2: fire retardant is the most pre-: process fire retardant after special pre-treatment;
S3: regeneration far infrared fire retardant polyester resin synthesis: by the p-phthalic acid after polyester bottle slice alcoholysis, ethylene glycol,
Catalyst by proportion puts in esterifying kettle after making beating, and glycolysis temperature controls between 250 DEG C, in still, Stress control exists
0.2MPa, after PET powder degradation is complete, adds negative ion far-infrared powder body solution, fire retardant treatment fluid, polycondensation catalyst,
Importing after being warming up to 260 DEG C in polycondensation vessel, it is 280 DEG C that condensation temperature controls, vacuum 10Pa, stops stirring after mechanical agitation 72h,
Cooled, pelletizing and being dried, prepares regeneration far infrared flame retardant polyester master batch;Described catalyst is zinc acetate;Described polycondensation is catalyzed
Agent is TiO2/SiO2 colloidal sol;Described fire retardant treatment fluid is triphenyl phosphate;
S4: polyester master particle is dried process, and makes Direct-spinning of PET Fiber section;
S5: Direct-spinning of PET Fiber section is carried out melt spinning, and through winding, drawing-off, crimp, cool down after cut-out, pack into
Storehouse.
In described step S3, p-phthalic acid, ethylene glycol, the volume mass ratio of catalyst are: 15ml:4ml:5g.
Addition negative ion far-infrared powder body, fire retardant treatment fluid, polycondensation catalyst and the matter of auxiliary agent in described step S3
Amount volume ratio is 4g:10ml:0.15g:0.022g
Described step S1 mid and far infrared powder body is made up of the raw material of following weight portion: Fe2O38 parts, SiO230 parts, Al2O3
30 parts, TiO260 parts, B2O322 parts, MgO 2.5 parts, ZrO20.8 part, ZnO 1.2 parts, NiO 0.04 part, CuO 2.2 parts.
Described step S4 is dried as condition as follows: first with the temperature drying 3.5 hours of 75 DEG C, then heat to 100
DEG C drying 1.5 hours, then it is warming up to 120 DEG C of blended dryings 1.5 hours, finally it is warming up to 145 DEG C of blended dryings 8 hours
More than and, criteria thus the drying time is not less than 16 hours.
In described step S5, the technological parameter of drawing-off is as follows: drafting multiple: 3.4 times;Drawing temperature: profit bathes 65 DEG C;Steam
Vapour 100 DEG C;Crispation number: 8-9/25mm;Heat setting temperature: 120 DEG C.
The performance of the polyester staple fiber of preparation, far emissivity is 0.88, and radiation wavelength 4 μm-18 μm, anion is sent out
Raw amount reaches 3170/cm3, fabric limited oxygen index reaches 36.8%.
Table 1 embodiment 1 far infrared powder physical and chemical index numerical value
Table 2 embodiment 1 far infrared powder compares with the physical and chemical index of pure tourmaline anion powder body
Test result shows, the multinomial physical and chemical index of powder body of the present invention is all superior than pure superfine tourmaline powder, especially
Whiteness, has obtained improving greatly, and the dyeing of textile is affected bigger by this.
The comparison of table 3 embodiment 1 its functional attributes
Be apparent from, embodiment 1 powder body in terms of various functions index also superior to existing pure tourmaline powder and list
One far-infrared powder.This complex function advantage has extremely important meaning to the manufacture process of fiber.It is known that it is functional
Powder body belongs to inorganic mineral, incompatible with macromolecular organic fiber material, along with the increase of addition in the fibre, chemical fibre
Intensity will be gradually lowered.Former functional textile, can only improve single index, wants to make fiber have complex function effect
Really, low-fiber intensity can only drop.By our improvements introduced in terms of powder body, can reach before identical addition
Putting, two kinds of functional parameters all reach the effect that domestic current mark is more excellent, and do not reduce the intensity index of chemical fibre, and this is novel
The outstanding advantages that composite superfine powder has.
Table 4 embodiment 1 natural radionuclide specific activity numerical value
In table 5 embodiment 1, Outreach services compares
Test data show, the composite superfine powder of present invention synthesis and the radioactive indicator of pure tourmaline powder are the least
In the radioactive level of Soils in Beijing Area, the numerical value specified well below construction material product, its range is not by any
Limiting, being actually this product does not has radioactivity.
After chemical modification and complex treatment, the efficient negative ion far-infrared ultrathin composite powder most typically of embodiment 1
Be characterized in that granule uniformly, narrow particle size distribution, the spherical rule body in class.We carry out sem analysis, result to approved product
See accompanying drawing 1.
Morphology microstructure is all in spherical particle, and the particle size distribution of overwhelming majority powder body is at 0.2~0.4 micron of model the narrowest
In enclosing.It is found that this shape characteristic can improve quality and its functional attributes of functional fiber from follow-up research,
Play the effect of protection equipment in process of production.
Table 6 is cut into slices key property
Test can only the results are shown in Table 7 with reference to the GB GBT 14464-2008 " terylene short fiber " of the short fine product of ordinary polyester.
Table 7 terylene short fiber quality test results
In order to investigate the negative ion far-infrared function persistency of fiber, we have investigated the attached of function powder in fiber and have deposited shape
State, to finding firm basis from inorganic particle existence in the fibre, we are to environment-friendly type regeneration negative ion far-infrared
The short fibre of function flame-resistant terylene is scanned Electronic Speculum (SEM) and analyzes, and can be clearly seen that superfine powder in each fiber
Distribution situation, fiber surface all shows that with section negative ion far-infrared powder dispersity is good.The addition of negative ion far-infrared powder body
Improve fiber surface roughness, the fabric construction that fiber finally prepares through twisting resultant yarn is loose, and porosity is washed than non-functional
The short fine product of synthetic fibre is high, and the short fine product of environment-friendly type regeneration negative ion far-infrared function flame-resistant terylene has good breathability.
Fiber product and the cloth product made thereafter have been carried out anion-generating capacity, far infrared transmission by respectively
Rate and the test of limited oxygen index, wherein anion-generating capacity is to be completed, far by China Man-made Fibre Industry TIA Product checking center
Infrared emittance is infrared by country and industrial electroheat product quality supervision and inspection center is tested, and limited oxygen index the results are shown in Table 8.
Table 8 negative ion far-infrared composite fiber product its functional attributes test result
Although the above-mentioned detailed description of the invention to the present invention is described, but not limit to scope
System, on the basis of technical scheme, those skilled in the art need not to pay that creative work can make is each
Plant amendment or deformation still within protection scope of the present invention.
Claims (7)
1. an environment-friendly type regeneration negative ion far-infrared function flame retardant polyester staple fibre, it is characterised in that: comprise the steps:
S1: the preparation of far-infrared powder liquid solution: use the modification that sand milling is combined with surfactant;
S2: fire retardant is the most pre-: process fire retardant after special pre-treatment;
S3: the synthesis of regeneration far infrared fire retardant polyester resin: by the p-phthalic acid after polyester bottle slice alcoholysis, ethylene glycol, catalysis
Agent puts in esterifying kettle in proportion after making beating, and glycolysis temperature controls between 245-260 DEG C, in still Stress control at 0.1-
0.3MPa, after PET powder degradation is complete, adds negative ion far-infrared powder body solution, fire retardant treatment fluid, polycondensation catalyst,
Importing after being warming up to 260 DEG C in polycondensation vessel, condensation temperature controls as 275-285 DEG C, and vacuum < 50Pa, after mechanical agitation 1h-96h
Stop stirring, cooled, pelletizing and be dried, prepare regeneration far infrared flame retardant polyester master batch;Described catalyst is zinc acetate;Described
Polycondensation catalyst is a kind of in TiO2/SiO2 colloidal sol, antimony glycol;Described fire retardant treatment fluid is TDE, ten bromines
One in diphenyl ether, triphenyl phosphate, triphenyl phosphate;
S4: polyester master particle is dried process, and makes Direct-spinning of PET Fiber section;
S5: Direct-spinning of PET Fiber section is carried out melt spinning, and through winding, drawing-off, crimp, cool down after cut-out, packaging and warehousing.
Environment-friendly type regeneration negative ion far-infrared function flame retardant polyester staple fibre the most according to claim 1, it is characterised in that:
In described step S3, p-phthalic acid, ethylene glycol, the volume mass ratio of catalyst are: 5-20ml:2-8ml:1-8g.
Environment-friendly type regeneration negative ion far-infrared function flame retardant polyester staple fibre the most according to claim 1, it is characterised in that:
Addition negative ion far-infrared powder body, fire retardant treatment fluid, polycondensation catalyst and the mass volume ratio of auxiliary agent in described step S3
For 2-10g:0.5-1.5ml:0.08-0.3g:0.012-0.05g.
Environment-friendly type regeneration negative ion far-infrared function flame retardant polyester staple fibre the most according to claim 1, it is characterised in that:
In described step S1, negative ion far-infrared powder body is made up of the raw material of following weight portion: Fe2O33.0-10 part, SiO2 27.5-50
Part, Al2O324-48 part, TiO230-90 part, B2O315.2-42 part, MgO 1-5 part, ZrO20.5-1.2 part, ZnO 0.1-2
Part, NiO 0.05-0.8 part, CuO 0.5-2.5 part.
Environment-friendly type regeneration negative ion far-infrared function flame retardant polyester staple fibre the most according to claim 1, it is characterised in that:
Described step S4 is dried as condition as follows: first with the temperature drying 3 of 70~80 DEG C~4 hours, then heat to 100 DEG C of bakings
Dry 1~2 hours, then be warming up to 120 DEG C of blended dryings 1~2 hours, be finally warming up to 145 DEG C of blended dryings 8 hours and
Above, criteria thus the drying time is not less than 16 hours.
Environment-friendly type regeneration negative ion far-infrared function flame retardant polyester staple fibre the most according to claim 1, it is characterised in that:
In described step S5, the technological parameter of drawing-off is as follows: drafting multiple: 3.4 times;Drawing temperature: profit bathes 65 DEG C;Steam 100 DEG C;
Crispation number: 8-9/25mm;Heat setting temperature: 120 DEG C.
Environment-friendly type regeneration negative ion far-infrared function flame retardant polyester staple fibre the most according to claim 1, it is characterised in that:
The performance of the polyester staple fiber of preparation, far emissivity is 0.88, and radiation wavelength 4 μm-18 μm, anion-generating capacity reaches
3170/cm3, fabric limited oxygen index reaches 36.8%.
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CN106757481A (en) * | 2016-12-27 | 2017-05-31 | 燕山大学 | Environment-friendly type negative ion far-infrared flame retardant polyester staple fibre and preparation method |
CN107740201A (en) * | 2017-11-03 | 2018-02-27 | 中科纺织研究院(青岛)有限公司 | A kind of negative-oxygen ion health function polyester fiber and preparation method thereof |
CN109913973A (en) * | 2019-03-12 | 2019-06-21 | 厦门旭纶成纺织科技有限公司 | A kind of fabric that can send out far infrared |
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CN112725937A (en) * | 2020-12-29 | 2021-04-30 | 河北宝盛纺织品有限公司 | Method for manufacturing fiber capable of generating negative ions |
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WO2019205513A1 (en) * | 2018-04-27 | 2019-10-31 | 常熟涤纶有限公司 | Preparation process for flame-retardant, colored and anti-infrared fiber |
CN109913973A (en) * | 2019-03-12 | 2019-06-21 | 厦门旭纶成纺织科技有限公司 | A kind of fabric that can send out far infrared |
CN110255904A (en) * | 2019-07-02 | 2019-09-20 | 浙江开尔新材料股份有限公司 | It can be except formaldehyde glaze slip, preparation method and the preparation method that formaldehyde enamel plate can be removed |
CN110255904B (en) * | 2019-07-02 | 2022-02-18 | 浙江开尔新材料股份有限公司 | Glaze slip capable of removing formaldehyde, preparation method and preparation method of enamel plate capable of removing formaldehyde |
CN111269408A (en) * | 2020-02-28 | 2020-06-12 | 浙江恒澜科技有限公司 | In-situ polymerization-based flame-retardant anti-dripping negative ion health-care polyester and preparation method thereof |
CN111826741A (en) * | 2020-07-26 | 2020-10-27 | 向自嫒 | Anion polyester fiber and fabric |
CN112725937A (en) * | 2020-12-29 | 2021-04-30 | 河北宝盛纺织品有限公司 | Method for manufacturing fiber capable of generating negative ions |
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