CN106336504A - Manufacturing method of flame-retardant anti-ageing PET (polyester) and fibers - Google Patents
Manufacturing method of flame-retardant anti-ageing PET (polyester) and fibers Download PDFInfo
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- CN106336504A CN106336504A CN201610782698.6A CN201610782698A CN106336504A CN 106336504 A CN106336504 A CN 106336504A CN 201610782698 A CN201610782698 A CN 201610782698A CN 106336504 A CN106336504 A CN 106336504A
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- 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
- C08G63/66—Polyesters containing oxygen in the form of ether groups
- C08G63/668—Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/672—Dicarboxylic acids and dihydroxy compounds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/10—Silicon-containing compounds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K7/00—Use of ingredients characterised by shape
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/34—Core-skin structure; Spinnerette packs therefor
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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
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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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C08K2201/00—Specific properties of additives
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- C08K2201/00—Specific properties of additives
- C08K2201/016—Additives defined by their aspect ratio
Abstract
The invention relates to a manufacturing method of flame-retardant anti-ageing PET (polyester) and fibers, and belongs to the technical field of manufacturing of functional fibers. The method comprises the following steps: mixing a halloysite nanotube, attapulgite crystals, aedelforsite raphioid fibers, a sodium bicarbonate aqueous solution, rutile type titanium dioxide and nano-montmorillonite; performing steaming reaction and microwave radiation; soaking the mixture into a citric acid solution to perform moisture absorption and dispersion; taking suspended materials and performing ultrasonic treatment; filtering, washing and drying the suspended materials on an upper layer; mixing the suspended materials on the upper layer, a phosphate flame retardant, antimonous oxide, a light stabilizer, an antioxidant, an ultraviolet light absorber and a coupling agent; melting the mixture and polyethylene glycol conventional PET to prepare flame-retardant anti-ageing PET; preparing the flame-retardant anti-ageing PET fibers from the obtained flame-retardant anti-ageing PET and the conventional PET. After the flame-retardant anti-ageing material is subjected to compound modification, the flame-retardant and anti-ageing effects of a skin layer and the brute force effect of a core layer are completely exerted, so the prepared PET and the PET fibers have high strength, high durability, flame retardance and ageing resistance.
Description
Technical field
The present invention relates to the manufacture method of a kind of flame-proof anti-aging pet and fiber, belong to functional fibre manufacturing technology field.
Background technology
Polyester (pet) fiber is to be with terephthalic acid (TPA) (pta) or dimethyl terephthalate (DMT) (dmt) and ethylene glycol (eg)
Raw material is through esterification or ester exchange fiber-forming polymer polyethylene terephthalate prepared through polycondensation reaction again
(pet) fiber, made through spinning, trade name terylene, is the first big kind of current synthetic fibers.Fiber macromolecular chain
Rigidity is larger, and elastic modelling quantity is high, and fiber is unlikely to deform, and it is good that its fabric has intensity, does not wrinkle after washing, can not press, strong very
Scrape, washable easily dry, be a kind of more satisfactory to take textile raw material.Pet fiber have in itself preferable uvioresistant, heat-resisting and
Light fastness, the industry that is used for that therefore gets more and more and outdoor field, such as tent, canopy, advertising cloth, casement, lamp house cloth etc..
In order to increase the service life in these fields, people generally carry out anti-aging process to it, and its processing mode is mainly pet fabric
Face coat and dipping, method is simple, and effect substantially, but is exposed to the weather or washed and easily come off, and persistence is poor.
The basic material of polyester is oil, while giving people the class rich and varied material conditions of offer by this pet fiber, also gives
The mankind have hidden a lot of disaster hidden-troubles.For safety it is necessary to improve the anti-flammability of pet fiber.Pet fabric face is usually taken
Coating and dipping fire proofing, give pet fabrics flame resistance performance, are equally that method is simple, effect substantially, but is exposed to the weather or washed
Wash and easily come off, persistence is poor.
Montmorillonite is the surface electronegative silicate lamella by nano thickness for the class, relies on the electrostatic interaction of interlayer and heap
The long-pending earthy mineral together constituting, the structure cell in its crystal structure is by one layer of alumina octahedral of folder in the middle of two-layer silicon-oxy tetrahedron
Body is constituted.There is one-dimensional layered nano-structure and the cation exchange characteristic of uniqueness, thus giving the many modifications of montmorillonite
May be with the expansion of application.Modified montmorillonite has a very strong adsorption capacity, good dispersive property, can be extensive
Application macromolecular material industry, as the additive of nanometer polymer macromolecular material, improves shock resistance, antifatigue, dimensionally stable
Property and gas barrier property etc., thus playing the effect strengthening polymer comprehensive physical performance, improve materiel machining performance simultaneously.
Application in the polymer can be added in polymer it is also possible to blending is added in melting.
The basic structural unit of attapulgite is bar-shaped, needle-like, fibrous monocrystal, and abbreviation concave convex rod is brilliant, attapulgite
The brilliant general ＜ of content 50% of middle rod, concave convex rod crystalline substance is about 0.5-5 μm, wide about 0.01-0.10 μm, and the brilliant surface of concave convex rod is covered with
Concavo-convex alternate groove, internal porous road, up to 500/more than g, water imbibition is strong, can reach more than 150%, Mohs for specific surface
Hardness 2-3 level, is heated to 700-800 DEG C, 5 grades of hardness ＞, and proportion is 2.05-2.32, adds in the plastic both as colouring agent,
There is reinforcement, fire-retardant, anti-aging again.
Rutile type titanium white both as colouring agent, has reinforcement, anti-aging, filling effect in rubber, plastics again.?
A small amount of rutile type titanium white is added in plastics, under solar radiation, sun-resistant, do not ftracture, nondiscolouring.Plastics system can be improved
The heat resistance of product, light resistance, weatherability, make the physical and chemical performance of plastic products be improved, and strengthen the mechanical strength of product,
Increase the service life.
Halloysite nanotubes are a kind of natural nano-materials with typical many walls nanotube shape structure, to cation,
Polar molecule etc. has a stronger adsorption capacity, and natural nano tubular structure and the property that is easily dispersed are so as to as a kind of
New enhancing by polymer is material modified very useful in thermoplastic.
Wollastonite raphioid fiber is a kind of anorthic system, thin platelike crystal, and aggregate is in radiation needle-like or threadiness, is heat
The preferably anti-aging packing material of plastic articles.Can improve product anti-aging, strengthen mobility and improve tensile strength.
Antimony oxide is the synergistic flame retardant of a excellent performance, has that synergistic is fire-retardant and anti-dripping effects, and outward appearance is
White powder.Be applied to polyurethane, neoprene, polyvinyl chloride, polypropylene, polyester etc., antimony oxide burning the initial stage,
It is melting first, form diaphragm isolation air in material surface, by the internal endothermic reaction, reduce ignition temperature.In high temperature
Under state, antimony oxide is gasified, and dilutes in the air oxygen concentration, thus playing fire retardation.
Tdbppe phosphate flame retardant, white or off-white color powder, for timber preservative, fire-retardant or manufacture fire retardant,
High thermal stability, resistance to migration, non-blooming.The good additive flame retardant with resin compatible.Due to containing two kinds of ignition-proof elements, having
Fire-retardant with plasticising dual-use function.Flame retarding efficiency is high, and persistently, consumption is less for effect.Be widely used in polyester pet, pbt, abs, pc,
The engineering plastics such as ppo, pc/abs, pc/pbt mixture.It is particularly suitable for the fire-retardant of transparent material.
Ultraviolet absorbent uv-327, can strong absorbing wavelength be the ultraviolet of 270-380 nanometer, chemical stability is good,
The heat endurance of product with antioxidant and with there being significant cooperative effect, can be significantly improved.Antioxidant dnp is to thermoplastic article
There is the antioxygenic property of brilliance, can effectively extend the useful life of product.Light stabilizer 770, can give product excellent family
Outer anti ageing property.
Scientific worker is directed to the defect that outdoor pet fiber exists for many years, has carried out substantial amounts of research, to being obtained
There is the high persistently flame-proof anti-aging pet fiber of intensity.
Content of the invention
It is an object of the invention to overcoming the shortcomings of that prior art exists, provide a kind of flame-proof anti-aging pet and fiber
Manufacture method.
The manufacture method of the flame-proof anti-aging pet that the present invention provides, using following steps:
A) galapectite that a diameter of 40-150nm of 0.3-0.5 part characterization parameter, length are 2-20 μm is taken to receive by mass fraction
Mitron, a length of 0.5-5 μm of 0.3-0.5 part characterization parameter, a width of 0.01-0.10 μm of concave convex rod crystalline substance, 0.8-1.2 part draw ratio is
14-16:0.5-1.5 wollastonite raphioid fiber, the aqueous solution of 4.0-6.0 part mass fraction 25-35% sodium acid carbonate, 0.3-0.5
Part rutile type titanium white, 0.2-0.4 part nano imvite, it is blended in stirring decatize in 150-170 DEG C of superheated steam reactor
Reaction 45-60min, radiates 2-4h in 300-400 DEG C of vacuum microwave, is then dipped in the lemon that 80-120 part mass fraction is 30%
In acid solution, vacuum moisture absorption is processed, and is heated to 60-95 DEG C of ultrasonic wave dispersion 0.5-1.5h, is stirred for disperseing 2-4h, takes after inhaling thoroughly
Suspension, at the deionized water ultrasonic wave at 75-85 DEG C with 60-100 part 3-5% containing mass fraction sodium tripolyphosphate dispersion liquid
Reason 25-35min, takes upper strata suspension to filter through 100-200 mesh, distilled water washes clean, and cleaning and drying obtains strengthening anti-aging
Agent；
B) take, by mass fraction, the enhancing age resister that step a) 8.0-12 part obtains, 6.0-10 part tdbppe phosphate,
1.0-3.0 part antimony oxide, 0.15-0.2 part 770 light stabilizer, 0.1-0.15 part dnp antioxidant, 0.4-0.6 part uv-327
Ultra-violet absorber, the kr-212 coupling agent mixing of 5-10 part mass fraction 10-20% concentration, in mixing under the conditions of 80-90 DEG C
With speed stirring reaction 45-60min of 250-350r/min in machine, 50-70 DEG C of vacuum drying obtains flame-proof anti-aging agent；
C) the flame-proof anti-aging agent that step b) 8.0-12 part obtains, 3.0-6.0 part molecular weight 0.5-1 ten thousand are taken by mass fraction
Polyethylene glycol, 10-18 part ethylene glycol, 70-80 DEG C of high-speed stirred 0.5-1.5h, obtain feature ethylene glycol；
D) by mass fraction, 8.0 parts of terephthalic acid (TPA)s and 5.0 parts of ethylene glycol are first esterified, in the diester of esterification
Change and add 1.0-2.0 part in section or class kettle by c) prepared feature ethylene glycol, until esterification, polycondensation reaction complete to make
Flame-proof anti-aging pet；
Or e) take the flame-proof anti-aging agent that step b) 8.0-12 part obtains, 2.0-5.0 part molecular weight 0.5-1 by mass fraction
Ten thousand polyethylene glycol, 80-120 part routine pet blended melting makes flame-proof anti-aging pet.
2. the manufacture method of the flame-proof anti-aging pet that the present invention provides, using following steps:
A) taking a diameter of 40-150nm of 0.4 part of characterization parameter, length by mass fraction is 2-20 μm of halloysite nanotubes,
A length of 0.5-5 μm of 0.4 part of characterization parameter, a width of 0.01-0.10 μm of concave convex rod crystalline substance, 1 part of draw ratio is 14-16:0.5-1.5 silicon ash
Stone raphioid fiber, the aqueous solution of 5.0 parts of mass fraction 30% sodium acid carbonates, 0.4 part of rutile type titanium white, 0.3 part of nanometer is covered
De- soil, is blended in stirring decatize reaction 53min in 160 DEG C of superheated steam reactors, radiates 3h in 350 DEG C of vacuum microwaves, then
It is dipped in vacuum moisture absorption in the citric acid solution that 100 parts of mass fractions are 30% to process, after inhaling thoroughly, be heated to 78 DEG C of ultrasonic waves dispersions
1h, is stirred for disperseing 3h, takes suspension, contains the deionized water of mass fraction 4% sodium tripolyphosphate dispersion liquid at 80 DEG C with 80 parts
Lower ultrasonication 30min, takes upper strata suspension to filter through 150 mesh, distilled water washes clean, cleaning and drying, obtains enhancing anti-
Aging dose；
B) take, by mass fraction, the enhancing age resister that 10 parts of step a) obtains, 8.0 parts of tdbppe phosphates, 2.0 part three
Aoxidize two antimony, 0.18 part of 770 light stabilizer, 0.13 part of dnp antioxidant, 0.5 part of uv-327 ultra-violet absorber, 8.0 parts of quality
The kr-212 coupling agent mixing of fraction 15% concentration, with the speed stirring reaction of 300r/min in mixer under the conditions of 85 DEG C
53min, 60 DEG C of vacuum dryings obtain flame-proof anti-aging agent；
C) the flame-proof anti-aging agent that 10 parts of step b) obtains, the poly- second two of 5.0 parts of molecular weight 0.5-1 ten thousand are taken by mass fraction
Alcohol, 14 parts of ethylene glycol, 75 DEG C of high-speed stirred 1h, obtain feature ethylene glycol；
D) by mass fraction, 8.0 parts of terephthalic acid (TPA)s and 5.0 parts of ethylene glycol are first esterified, in the diester of esterification
Change and add 1.5 parts in section or class kettle by c) prepared feature ethylene glycol, until esterification, polycondensation reaction complete to make fire-retardant
Anti-aging pet；
Or e) take the flame-proof anti-aging agent that 10 parts of step b) obtains, the poly- second of 4.0 parts of molecular weight 0.5-1 ten thousand by mass fraction
Glycol, 100 parts of conventional pet blended meltings make flame-proof anti-aging pet.
3. the manufacture method of the flame-proof anti-aging pet fiber that the present invention provides, using following steps:
A) galapectite that a diameter of 40-150nm of 0.3-0.5 part characterization parameter, length are 2-20 μm is taken to receive by mass fraction
Mitron, a length of 0.5-5 μm of 0.3-0.5 part characterization parameter, a width of 0.01-0.10 μm of concave convex rod crystalline substance, 0.8-1.2 part draw ratio is
14-16:0.5-1.5 wollastonite raphioid fiber, the aqueous solution of 4.0-6.0 part mass fraction 25-35% sodium acid carbonate, 0.3-0.5
Part rutile type titanium white, 0.2-0.4 part nano imvite, it is blended in stirring decatize in 150-170 DEG C of superheated steam reactor
Reaction 45-60min, radiates 2-4h in 300-400 DEG C of vacuum microwave, is then dipped in the lemon that 80-120 part mass fraction is 30%
In acid solution, vacuum moisture absorption is processed, and is heated to 60-95 DEG C of ultrasonic wave dispersion 0.5-1.5h, is stirred for disperseing 2-4h, takes after inhaling thoroughly
Suspension, at the deionized water ultrasonic wave at 75-85 DEG C with 60-100 part 3-5% containing mass fraction sodium tripolyphosphate dispersion liquid
Reason 25-35min, takes upper strata suspension to filter through 100-200 mesh, distilled water washes clean, and cleaning and drying obtains strengthening anti-aging
Agent；
B) take, by mass fraction, the enhancing age resister that step a) 8.0-12 part obtains, 6.0-10 part tdbppe phosphate,
1.0-3.0 part antimony oxide, 0.15-0.2 part 770 light stabilizer, 0.1-0.15 part dnp antioxidant, 0.4-0.6 part uv-327
Ultra-violet absorber, the kr-212 coupling agent mixing of 5.0-10 part mass fraction 10-20% concentration, mixed under the conditions of 80-90 DEG C
With speed stirring reaction 45-60min of 250-350r/min in conjunction machine, 50-70 DEG C of vacuum drying obtains flame-proof anti-aging agent；
C) the flame-proof anti-aging agent that step b) 8.0-12 part obtains, 3.0-6.0 part molecular weight 0.5-1 ten thousand are taken by mass fraction
Polyethylene glycol, 10-18 part ethylene glycol, 70-80 DEG C of high-speed stirred 0.5-1.5h, obtain feature ethylene glycol；
D) by mass fraction, 8.0 parts of terephthalic acid (TPA)s and 5.0 parts of ethylene glycol are first esterified, in the diester of esterification
Change and add 1.0-2.0 part in section or class kettle by c) prepared feature ethylene glycol, until esterification, polycondensation reaction complete to make
Flame-proof anti-aging pet；
Or e) take the flame-proof anti-aging agent that step b) 8.0-12 part obtains, 2.0-5.0 part molecular weight 0.5-1 by mass fraction
Ten thousand polyethylene glycol, 80-120 part routine pet blended melting makes flame-proof anti-aging pet.
F) the flame-proof anti-aging pet obtaining step d) or step e) is cortex and conventional pet is sandwich layer, and melting is combined makes
Become core-skin type lasting flame-proof anti-aging pet fiber.
Compared with prior art, the present invention, modified for flame-proof anti-aging Material cladding, is dispersed in microfibril form
Inside pet, make, through melting, the core-skin type lasting flame-proof anti-aging pet fiber that flame-proof anti-aging pet is cortex, give full play to skin
The flame-proof anti-aging of layer and the forceful action of sandwich layer, pet the and pet fiber made has the high persistently flame-proof anti-aging of intensity
Energy.
Specific embodiment
Below in conjunction with specific embodiment, the present invention will be described in detail: the flame-proof anti-aging pet's that the present invention provides
Manufacture method, using following steps:
A) galapectite that a diameter of 40-150nm of 0.3-0.5 part characterization parameter, length are 2-20 μm is taken to receive by mass fraction
Mitron, a length of 0.5-5 μm of 0.3-0.5 part characterization parameter, a width of 0.01-0.10 μm of concave convex rod crystalline substance, 0.8-1.2 part draw ratio is
14-16:0.5-1.5 wollastonite raphioid fiber, the aqueous solution of 4.0-6.0 part mass fraction 25-35% sodium acid carbonate, 0.3-0.5
Part rutile type titanium white, 0.2-0.4 part nano imvite, it is blended in stirring decatize in 150-170 DEG C of superheated steam reactor
Reaction 45-60min, radiates 2-4h in 300-400 DEG C of vacuum microwave, is then dipped in the lemon that 80-120 part mass fraction is 30%
In acid solution, vacuum moisture absorption is processed, and is heated to 60-95 DEG C of ultrasonic wave dispersion 0.5-1.5h, is stirred for disperseing 2-4h, takes after inhaling thoroughly
Suspension, at the deionized water ultrasonic wave at 75-85 DEG C with 60-100 part 3-5% containing mass fraction sodium tripolyphosphate dispersion liquid
Reason 25-35min, takes upper strata suspension to filter through 100-200 mesh, distilled water washes clean, and cleaning and drying obtains strengthening anti-aging
Agent；
B) take, by mass fraction, the enhancing age resister that step a) 8.0-12 part obtains, 6.0-10 part tdbppe phosphate,
1.0-3.0 part antimony oxide, 0.15-0.2 part 770 light stabilizer, 0.1-0.15 part dnp antioxidant, 0.4-0.6 part uv-327
Ultra-violet absorber, the kr-212 coupling agent mixing of 5.0-10 part mass fraction 10-20% concentration, mixed under the conditions of 80-90 DEG C
With speed stirring reaction 45-60min of 250-350r/min in conjunction machine, 50-70 DEG C of vacuum drying obtains flame-proof anti-aging agent；
C) the flame-proof anti-aging agent that step b) 8.0-12 part obtains, 3.0-6.0 part molecular weight 0.5-1 ten thousand are taken by mass fraction
Polyethylene glycol, 10-18 part ethylene glycol, 70-80 DEG C of high-speed stirred 0.5-1.5h, obtain feature ethylene glycol；
D) by mass fraction, 8.0 parts of terephthalic acid (TPA)s and 5.0 parts of ethylene glycol are first esterified, in the diester of esterification
Change and add 1.0-2.0 part in section or class kettle by c) prepared feature ethylene glycol, until esterification, polycondensation reaction complete to make
Flame-proof anti-aging pet；
Or e) take the flame-proof anti-aging agent that step b) 8.0-12 part obtains, 2.0-5.0 part molecular weight 0.5-1 by mass fraction
Ten thousand polyethylene glycol, 80-120 part routine pet blended melting makes flame-proof anti-aging pet.
The manufacture method of the flame-proof anti-aging pet fiber that the present invention provides, using following steps:
A) galapectite that a diameter of 40-150nm of 0.3-0.5 part characterization parameter, length are 2-20 μm is taken to receive by mass fraction
Mitron, a length of 0.5-5 μm of 0.3-0.5 part characterization parameter, a width of 0.01-0.10 μm of concave convex rod crystalline substance, 0.8-1.2 part draw ratio is
14-16:0.5-1.5 wollastonite raphioid fiber, the aqueous solution of 4.0-6.0 part mass fraction 25-35% sodium acid carbonate, 0.3-0.5
Part rutile type titanium white, 0.2-0.4 part nano imvite, it is blended in stirring decatize in 150-170 DEG C of superheated steam reactor
Reaction 45-60min, radiates 2-4h in 300-400 DEG C of vacuum microwave, is then dipped in the lemon that 80-120 part mass fraction is 30%
In acid solution, vacuum moisture absorption is processed, and is heated to 60-95 DEG C of ultrasonic wave dispersion 0.5-1.5h, is stirred for disperseing 2-4h, takes after inhaling thoroughly
Suspension, at the deionized water ultrasonic wave at 75-85 DEG C with 60-100 part 3-5% containing mass fraction sodium tripolyphosphate dispersion liquid
Reason 25-35min, takes upper strata suspension to filter through 100-200 mesh, distilled water washes clean, and cleaning and drying obtains strengthening anti-aging
Agent；
B) take, by mass fraction, the enhancing age resister that step a) 8.0-12 part obtains, 6.0-10 part tdbppe phosphate,
1.0-3.0 part antimony oxide, 0.15-0.2 part 770 light stabilizer, 0.1-0.15 part dnp antioxidant, 0.4-0.6 part uv-327
Ultra-violet absorber, the kr-212 coupling agent mixing of 5.0-10 part mass fraction 10-20% concentration, mixed under the conditions of 80-90 DEG C
With speed stirring reaction 45-60min of 250-350r/min in conjunction machine, 50-70 DEG C of vacuum drying obtains flame-proof anti-aging agent；
C) the flame-proof anti-aging agent that step b) 8.0-12 part obtains, 3.0-6.0 part molecular weight 0.5-1 ten thousand are taken by mass fraction
Polyethylene glycol, 10-18 part ethylene glycol, 70-80 DEG C of high-speed stirred 0.5-1.5h, obtain feature ethylene glycol；
D) by mass fraction, 8.0 parts of terephthalic acid (TPA)s and 5.0 parts of ethylene glycol are first esterified, in the diester of esterification
Change and add 1.0-2.0 part in section or class kettle by c) prepared feature ethylene glycol, until esterification, polycondensation reaction complete to make
Flame-proof anti-aging pet；
Or e) take the flame-proof anti-aging agent that step b) 8.0-12 part obtains, 2.0-5.0 part molecular weight 0.5-1 by mass fraction
Ten thousand polyethylene glycol, 80-120 part routine pet blended melting makes flame-proof anti-aging pet.
F) the flame-proof anti-aging pet obtaining step d) or step e) is cortex and conventional pet is sandwich layer, and melting is combined makes
Become core-skin type lasting flame-proof anti-aging pet fiber.
Embodiment 1: a kind of manufacture method of flame-proof anti-aging pet, using following steps:
A) taking a diameter of 40-150nm of 0.3 part of characterization parameter, length by mass fraction is 2-20 μm of halloysite nanotubes,
A length of 0.5-5 μm of 0.3 part of characterization parameter, a width of 0.01-0.10 μm of concave convex rod crystalline substance, 0.8 part of draw ratio is 14-16:0.5-1.5 silicon
Lime stone raphioid fiber, the aqueous solution of 4.0 parts of mass fraction 25% sodium acid carbonates, 0.3 part of rutile type titanium white, 0.2 part of nanometer
Montmorillonite, is blended in stirring decatize reaction 45min in 150 DEG C of superheated steam reactors, radiates 2h in 300 DEG C of vacuum microwaves, so
It is dipped in vacuum moisture absorption in the citric acid solution that 80 parts of mass fractions are 30% afterwards to process, after inhaling thoroughly, be heated to 60 DEG C of ultrasonic waves dispersions
0.5h, is stirred for disperseing 2h, takes suspension, contains the deionized waters of mass fraction 3% sodium tripolyphosphate dispersion liquid 75 with 60 parts
Ultrasonication 25min at DEG C, takes upper strata suspension to filter through 100 mesh, distilled water washes clean, and cleaning and drying is strengthened
Age resister；
B) take, by mass fraction, the enhancing age resister that 8.0 parts of step a) obtains, 6.0 parts of tdbppe phosphates, 1.0 part three
Aoxidize two antimony, 0.15 part of 770 light stabilizer, 0.1 part of dnp antioxidant, 0.4 part of uv-327 ultra-violet absorber, 5.0 parts of quality are divided
The kr-212 coupling agent mixing of several 10% concentration, with the speed stirring reaction of 250r/min in mixer under the conditions of 80 DEG C
45min, 50 DEG C of vacuum dryings obtain flame-proof anti-aging agent；
C) the flame-proof anti-aging agent that 8.0 parts of step b) obtains, the poly- second of 3.0 parts of molecular weight 0.5-1 ten thousand are taken by mass fraction
Glycol, 10-18 part ethylene glycol, 70 DEG C of high-speed stirred 0.5h, obtain feature ethylene glycol；
D) by mass fraction, 8.0 parts of terephthalic acid (TPA)s and 5.0 parts of ethylene glycol are first esterified, in the diester of esterification
Change and add 1.0 parts in section or class kettle by c) prepared feature ethylene glycol, until esterification, polycondensation reaction complete to make fire-retardant
Anti-aging pet；
Or e) taking, by mass fraction, the flame-proof anti-aging agent that 8.0 parts of step b) obtains, 2.0 parts of molecular weight 0.5-1's ten thousand is poly-
Ethylene glycol, 80 parts of conventional pet blended meltings make flame-proof anti-aging pet.
A kind of manufacture method of flame-proof anti-aging pet fiber, using following steps:
A) taking a diameter of 40-150nm of 0.3 part of characterization parameter, length by mass fraction is 2-20 μm of halloysite nanotubes,
A length of 0.5-5 μm of 0.3 part of characterization parameter, a width of 0.01-0.10 μm of concave convex rod crystalline substance, 0.8 part of draw ratio is 14-16:0.5-1.5 silicon
Lime stone raphioid fiber, the aqueous solution of 4 parts of mass fraction 25% sodium acid carbonates, 0.3 part of rutile type titanium white, 0.2 part of nanometer is covered
De- soil, is blended in stirring decatize reaction 45min in 150 DEG C of superheated steam reactors, radiates 2h in 300 DEG C of vacuum microwaves, then
It is dipped in vacuum moisture absorption in the citric acid solution that 80 parts of mass fractions are 30% to process, after inhaling thoroughly, be heated to 60 DEG C of ultrasonic waves dispersions
0.5h, is stirred for disperseing 2h, takes suspension, contains the deionized waters of mass fraction 3% sodium tripolyphosphate dispersion liquid 75 with 60 parts
Ultrasonication 25min at DEG C, takes upper strata suspension to filter through 100 mesh, distilled water washes clean, and cleaning and drying is strengthened
Age resister；
B) take, by mass fraction, the enhancing age resister that 8.0 parts of step a) obtains, 6.0 parts of tdbppe phosphates, 1.0 part three
Aoxidize two antimony, 0.15 part of 770 light stabilizer, 0.1 part of dnp antioxidant, 0.4 part of uv-327 ultra-violet absorber, 5.0 parts of quality are divided
The kr-212 coupling agent mixing of several 10% concentration, with the speed stirring reaction of 250r/min in mixer under the conditions of 80 DEG C
45min, 50 DEG C of vacuum dryings obtain flame-proof anti-aging agent；
C) the flame-proof anti-aging agent that 8.0 parts of step b) obtains, the poly- second of 3.0 parts of molecular weight 0.5-1 ten thousand are taken by mass fraction
Glycol, 10-18 part ethylene glycol, 70 DEG C of high-speed stirred 0.5h, obtain feature ethylene glycol；
D) by mass fraction, 8.0 parts of terephthalic acid (TPA)s and 5.0 parts of ethylene glycol are first esterified, in the diester of esterification
Change and add 1.0 parts in section or class kettle by c) prepared feature ethylene glycol, until esterification, polycondensation reaction complete to make fire-retardant
Anti-aging pet；
Or e) take, by mass fraction, the flame-proof anti-aging agent that 8.0 parts of step b) obtains, the poly- second of 2.0 parts of molecular weight 0.5-1 ten thousand
Glycol, 80 parts of conventional pet blended meltings make flame-proof anti-aging pet.
F) the flame-proof anti-aging pet obtaining step d) or step e) is cortex and conventional pet is sandwich layer, and melting is combined makes
Become core-skin type lasting flame-proof anti-aging pet fiber.
Embodiment 2: a kind of manufacture method of flame-proof anti-aging pet, using following steps:
A) taking a diameter of 40-150nm of 0.4 part of characterization parameter, length by mass fraction is 2-20 μm of halloysite nanotubes,
A length of 0.5-5 μm of 0.4 part of characterization parameter, a width of 0.01-0.10 μm of concave convex rod crystalline substance, 1 part of draw ratio is 14-16:0.5-1.5 silicon ash
Stone raphioid fiber, the aqueous solution of 5 parts of mass fraction 30% sodium acid carbonates, 0.4 part of rutile type titanium white, 0.3 part of nanometer is covered and is taken off
Soil, is blended in stirring decatize reaction 53min in 160 DEG C of superheated steam reactors, radiates 3h in 350 DEG C of vacuum microwaves, then soak
In part 100 mass fraction be 30% citric acid solution in vacuum moisture absorption process, be heated to 78 DEG C of ultrasonic waves dispersion 1h after inhaling thoroughly,
It is stirred for disperseing 3h, takes suspension, the deionized water containing mass fraction 4% sodium tripolyphosphate dispersion liquid with 80 parts is super at 80 DEG C
Sonicated 30min, takes upper strata suspension to filter through 150 mesh, distilled water washes clean, cleaning and drying, obtains strengthening anti-aging
Agent；
B) take, by mass fraction, the enhancing age resister that 10 parts of step a) obtains, 8.0 parts of tdbppe phosphates, 2.0 part three
Aoxidize two antimony, 0.18 part of 770 light stabilizer, 0.13 part of dnp antioxidant, 0.5 part of uv-327 ultra-violet absorber, 8.0 parts of quality
The kr-212 coupling agent mixing of fraction 15% concentration, with the speed stirring reaction of 300r/min in mixer under the conditions of 85 DEG C
53min, 60 DEG C of vacuum dryings obtain flame-proof anti-aging agent；
C) the flame-proof anti-aging agent that 10 parts of step b) obtains, the poly- second two of 5.0 parts of molecular weight 0.5-1 ten thousand are taken by mass fraction
Alcohol, 14 parts of ethylene glycol, 75 DEG C of high-speed stirred 1h, obtain feature ethylene glycol；
D) by mass fraction, 8.0 parts of terephthalic acid (TPA)s and 5.0 parts of ethylene glycol are first esterified, in the diester of esterification
Change and add 1.5 parts in section or class kettle by c) prepared feature ethylene glycol, until esterification, polycondensation reaction complete to make fire-retardant
Anti-aging pet；
Or e) take the flame-proof anti-aging agent that 10 parts of step b) obtains, the poly- second two of 4 parts of molecular weight 0.5-1 ten thousand by mass fraction
Alcohol, 100 parts of conventional pet blended meltings make flame-proof anti-aging pet.
A kind of manufacture method of flame-proof anti-aging pet fiber, using following steps:
A) taking a diameter of 40-150nm of 0.4 part of characterization parameter, length by mass fraction is 2-20 μm of halloysite nanotubes,
A length of 0.5-5 μm of 0.4 part of characterization parameter, a width of 0.01-0.10 μm of concave convex rod crystalline substance, 1 part of draw ratio is 14-16:0.5-1.5 silicon ash
Stone raphioid fiber, the aqueous solution of 5 parts of mass fraction 30% sodium acid carbonates, 0.4 part of rutile type titanium white, 0.3 part of nanometer is covered and is taken off
Soil, is blended in stirring decatize reaction 53min in 160 DEG C of superheated steam reactors, radiates 3h in 350 DEG C of vacuum microwaves, then soak
In part 100 mass fraction be 30% citric acid solution in vacuum moisture absorption process, be heated to 78 DEG C of ultrasonic waves dispersion 1h after inhaling thoroughly,
It is stirred for disperseing 3h, takes suspension, the deionized water containing mass fraction 4% sodium tripolyphosphate dispersion liquid with 80 parts is super at 80 DEG C
Sonicated 30min, takes upper strata suspension to filter through 150 mesh, distilled water washes clean, cleaning and drying, obtains strengthening anti-aging
Agent；
B) take, by mass fraction, the enhancing age resister that 10 parts of step a) obtains, 8.0 parts of tdbppe phosphates, 2.0 part three
Aoxidize two antimony, 0.18 part of 770 light stabilizer, 0.13 part of dnp antioxidant, 0.5 part of uv-327 ultra-violet absorber, 8.0 parts of quality
The kr-212 coupling agent mixing of fraction 15% concentration, with the speed stirring reaction of 300r/min in mixer under the conditions of 85 DEG C
53min, 60 DEG C of vacuum dryings obtain flame-proof anti-aging agent；
C) the flame-proof anti-aging agent that 10 parts of step b) obtains, the poly- second two of 5.0 parts of molecular weight 0.5-1 ten thousand are taken by mass fraction
Alcohol, 14 parts of ethylene glycol, 75 DEG C of high-speed stirred 1h, obtain feature ethylene glycol；
D) by mass fraction, 8.0 parts of terephthalic acid (TPA)s and 5.0 parts of ethylene glycol are first esterified, in the diester of esterification
Change and add 1.5 parts in section or class kettle by c) prepared feature ethylene glycol, until esterification, polycondensation reaction complete to make fire-retardant
Anti-aging pet；
Or e) take the flame-proof anti-aging agent that 10 parts of step b) obtains, the second that 4.0 parts of molecular weight 0.5-1 ten thousand gather by mass fraction
Glycol, 100 parts of conventional pet blended meltings make flame-proof anti-aging pet.
F) the flame-proof anti-aging pet obtaining step d) or step e) is cortex and conventional pet is sandwich layer, and melting is combined makes
Become core-skin type lasting flame-proof anti-aging pet fiber.
Embodiment 3: a kind of manufacture method of flame-proof anti-aging pet, using following steps:
A) taking a diameter of 40-150nm of 0.5 part of characterization parameter, length by mass fraction is 2-20 μm of halloysite nanotubes,
A length of 0.5-5 μm of 0.5 part of characterization parameter, a width of 0.01-0.10 μm of concave convex rod crystalline substance, 1.2 parts of draw ratios are 14-16:0.5-1.5 silicon
Lime stone raphioid fiber, the aqueous solution of 6 parts of mass fraction 35% sodium acid carbonates, 0.5 part of rutile type titanium white, 0.4 part of nanometer is covered
De- soil, is blended in stirring decatize reaction 60min in 170 DEG C of superheated steam reactors, radiates 4h in 400 DEG C of vacuum microwaves, then
It is dipped in vacuum moisture absorption in the citric acid solution that 120 parts of mass fractions are 30% to process, after inhaling thoroughly, be heated to 95 DEG C of ultrasonic waves dispersions
1.5h, is stirred for disperseing 4h, takes suspension, contains the deionized waters of mass fraction 5% sodium tripolyphosphate dispersion liquid 85 with 100 parts
Ultrasonication 35min at DEG C, takes upper strata suspension to filter through 200 mesh, distilled water washes clean, and cleaning and drying is strengthened
Age resister；
B) the enhancing age resister that 12 parts of step a) obtains, 10 parts of tdbppe phosphates, 3.0 part of three oxygen are taken by mass fraction
Change two antimony, 0.2 part of 770 light stabilizer, 0.15 part of dnp antioxidant, 0.6 part of uv-327 ultra-violet absorber, 10 parts of mass fractions
The kr-212 coupling agent mixing of 20% concentration, with speed stirring reaction 60min of 350r/min in mixer under the conditions of 90 DEG C,
70 DEG C of vacuum dryings obtain flame-proof anti-aging agent；
C) the flame-proof anti-aging agent that 12 parts of step b) obtains, the poly- second two of 6.0 parts of molecular weight 0.5-1 ten thousand are taken by mass fraction
Alcohol, 18 parts of ethylene glycol, 80 DEG C of high-speed stirred 1.5h, obtain feature ethylene glycol；
D) by mass fraction, 8.0 parts of terephthalic acid (TPA)s and 5.0 parts of ethylene glycol are first esterified, in the diester of esterification
Change and add 2.0 parts in section or class kettle by c) prepared feature ethylene glycol, until esterification, polycondensation reaction complete to make fire-retardant
Anti-aging pet；
Or e) take the flame-proof anti-aging agent that 12 parts of step b) obtains, the poly- second of 5.0 parts of molecular weight 0.5-1 ten thousand by mass fraction
Glycol, 120 parts of conventional pet blended meltings make flame-proof anti-aging pet.
A kind of manufacture method of flame-proof anti-aging pet fiber, using following steps:
A) taking a diameter of 40-150nm of 0.5 part of characterization parameter, length by mass fraction is 2-20 μm of halloysite nanotubes,
A length of 0.5-5 μm of 0.5 part of characterization parameter, a width of 0.01-0.10 μm of concave convex rod crystalline substance, 1.2 parts of draw ratios are 14-16:0.5-1.5 silicon
Lime stone raphioid fiber, the aqueous solution of 6 parts of mass fraction 35% sodium acid carbonates, 0.5 part of rutile type titanium white, 0.4 part of nanometer is covered
De- soil, is blended in stirring decatize reaction 60min in 170 DEG C of superheated steam reactors, radiates 4h in 400 DEG C of vacuum microwaves, then
It is dipped in vacuum moisture absorption in the citric acid solution that 120 parts of mass fractions are 30% to process, after inhaling thoroughly, be heated to 95 DEG C of ultrasonic waves dispersions
1.5h, is stirred for disperseing 4h, takes suspension, contains the deionized waters of mass fraction 5% sodium tripolyphosphate dispersion liquid 85 with 100 parts
Ultrasonication 35min at DEG C, takes upper strata suspension to filter through 200 mesh, distilled water washes clean, and cleaning and drying is strengthened
Age resister；
B) the enhancing age resister that 12 parts of step a) obtains, 10 parts of tdbppe phosphates, 3.0 part of three oxygen are taken by mass fraction
Change two antimony, 0.2 part of 770 light stabilizer, 0.15 part of dnp antioxidant, 0.6 part of uv-327 ultra-violet absorber, 10 parts of mass fractions
The kr-212 coupling agent mixing of 20% concentration, with speed stirring reaction 60min of 350r/min in mixer under the conditions of 90 DEG C,
70 DEG C of vacuum dryings obtain flame-proof anti-aging agent；
C) take, by mass fraction, the flame-proof anti-aging agent that 12 parts of step b) obtains, the poly- second two of 6.0 parts of molecular weight 0.5-1 ten thousand
Alcohol, 18 parts of ethylene glycol, 80 DEG C of high-speed stirred 1.5h, obtain feature ethylene glycol；
D) by mass fraction, 8.0 parts of terephthalic acid (TPA)s and 5.0 parts of ethylene glycol are first esterified, in the diester of esterification
Change and add 2.0 parts in section or class kettle by c) prepared feature ethylene glycol, until esterification, polycondensation reaction complete to make fire-retardant
Anti-aging pet；
Or e) take the flame-proof anti-aging agent that 12 parts of step b) obtains, the poly- second of 5.0 parts of molecular weight 0.5-1 ten thousand by mass fraction
Glycol, 120 parts of conventional pet blended meltings make flame-proof anti-aging pet.
F) the flame-proof anti-aging pet obtaining step d) or step e) is cortex and conventional pet is sandwich layer, and melting is combined makes
Become core-skin type lasting flame-proof anti-aging pet fiber.
Embodiment of the present invention is not limited to embodiment described above, by aforementioned disclosed number range, just
Arbitrarily replaced in specific embodiment, such that it is able to obtain numerous embodiment, this is not enumerated.
Claims (3)
1. a kind of manufacture method of flame-proof anti-aging pet is it is characterised in that this manufacture method adopts following steps:
A) take, by mass fraction, the halloysite nanotubes that a diameter of 40-150nm of 0.3-0.5 part characterization parameter, length are 2-20 μm,
A length of 0.5-5 μm of 0.3-0.5 part characterization parameter, a width of 0.01-0.10 μm of concave convex rod crystalline substance, 0.8-1.2 part draw ratio is 14-16:
0.5-1.5 wollastonite raphioid fiber, the aqueous solution of 4.0-6.0 part mass fraction 25-35% sodium acid carbonate, 0.3-0.5 part golden red
Stone-type titanium dioxide, 0.2-0.4 part nano imvite, it is blended in stirring decatize reaction 45- in 150-170 DEG C of superheated steam reactor
60min, radiates 2-4h in 300-400 DEG C of vacuum microwave, is then dipped in the citric acid solution that 80-120 part mass fraction is 30%
Middle vacuum moisture absorption is processed, and is heated to 60-95 DEG C of ultrasonic wave dispersion 0.5-1.5h, is stirred for disperseing 2-4h, takes suspension after inhaling thoroughly,
With the deionized water of 60-100 part 3-5% containing mass fraction sodium tripolyphosphate dispersion liquid at 75-85 DEG C ultrasonication 25-
35min, takes upper strata suspension to filter through 100-200 mesh, distilled water washes clean, and cleaning and drying obtains strengthening age resister；
B) the enhancing age resister that step a) 8.0-12 part obtains, 6.0-10 part tdbppe phosphate, 1.0- are taken by mass fraction
3.0 parts of antimony oxides, 0.15-0.2 part 770 light stabilizer, 0.1-0.15 part dnp antioxidant, 0.4-0.6 part uv-327 ultraviolet
Light absorbers, the kr-212 coupling agent mixing of 5.0-10 part mass fraction 10-20% concentration, in mixer under the conditions of 80-90 DEG C
In flame-proof anti-aging agent is obtained with speed stirring reaction 45-60min of 250-350r/min, 50-70 DEG C of vacuum drying；
C) take, by mass fraction, the flame-proof anti-aging agent that step b) 8.0-12 part obtains, 3.0-6.0 part molecular weight 0.5-1's ten thousand is poly-
Ethylene glycol, 10-18 part ethylene glycol, 70-80 DEG C of high-speed stirred 0.5-1.5h, obtain feature ethylene glycol；
D) by mass fraction, 8.0 parts of terephthalic acid (TPA)s and 5.0 parts of ethylene glycol are first esterified, at class section of esterification
Or add 1.0-2.0 part in class kettle by c) prepared feature ethylene glycol, until esterification, polycondensation reaction complete to make fire-retardant
Anti-aging pet；
Or e) taking, by mass fraction, the flame-proof anti-aging agent that step b) 8.0-12 part obtains, 2.0-5.0 part molecular weight 0.5-1 ten thousand gathers
Ethylene glycol, 80-120 part routine pet blended melting make flame-proof anti-aging pet.
2. a kind of manufacture method of flame-proof anti-aging pet is it is characterised in that this manufacture method adopts following steps:
A) taking a diameter of 40-150nm of 0.4 part of characterization parameter, length by mass fraction is 2-20 μm of halloysite nanotubes, 0.4
A length of 0.5-5 μm of characterization parameter of part, a width of 0.01-0.10 μm of concave convex rod crystalline substance, 1 part of draw ratio is 14-16:0.5-1.5 wollastonite
Raphioid fiber, the aqueous solution of 5 parts of mass fraction 30% sodium acid carbonates, 0.4 part of rutile type titanium white, 0.3 part of nano imvite,
It is blended in stirring decatize reaction 53min in 160 DEG C of superheated steam reactors, radiate 3h in 350 DEG C of vacuum microwaves, be then dipped in
100 parts of mass fractions be 30% citric acid solution in vacuum moisture absorption process, be heated to 78 DEG C of ultrasonic waves dispersion 1h after inhaling thoroughly, then
Dispersed with stirring 3h, takes suspension, and the deionized water containing mass fraction 4% sodium tripolyphosphate dispersion liquid with 80 parts is ultrasonic at 80 DEG C
Ripple processes 30min, takes upper strata suspension to filter through 150 mesh, distilled water washes clean, cleaning and drying, obtains strengthening age resister；
B) the enhancing age resister that 10 parts of step a) obtains, 8.0 parts of tdbppe phosphates, 2.0 part of three oxidation are taken by mass fraction
Two antimony, 0.18 part of 770 light stabilizer, 0.13 part of dnp antioxidant, 0.5 part of uv-327 ultra-violet absorber, 8.0 parts of mass fractions
The kr-212 coupling agent mixing of 15% concentration, with speed stirring reaction 53min of 300r/min in mixer under the conditions of 85 DEG C,
60 DEG C of vacuum dryings obtain flame-proof anti-aging agent；
C) take, by mass fraction, the flame-proof anti-aging agent that 10 parts of step b) obtains, the polyethylene glycol of 5.0 parts of molecular weight 0.5-1 ten thousand,
14 parts of ethylene glycol, 75 DEG C of high-speed stirred 1h, obtain feature ethylene glycol；
D) by mass fraction, 8.0 parts of terephthalic acid (TPA)s and 5.0 parts of ethylene glycol are first esterified, at class section of esterification
Or add 1.5 parts in class kettle by c) prepared feature ethylene glycol, until esterification, polycondensation reaction complete to make fire-retardant anti-ageing
Change pet；
Or e) take the flame-proof anti-aging agent that 10 parts of step b) obtains, the poly- second two of 4.0 parts of molecular weight 0.5-1 ten thousand by mass fraction
Alcohol, 100 parts of conventional pet blended meltings make flame-proof anti-aging pet.
3. a kind of manufacture method of flame-proof anti-aging pet fiber is it is characterised in that this manufacture method adopts following steps:
A) take, by mass fraction, the halloysite nanotubes that a diameter of 40-150nm of 0.3-0.5 part characterization parameter, length are 2-20 μm,
A length of 0.5-5 μm of 0.3-0.5 part characterization parameter, a width of 0.01-0.10 μm of concave convex rod crystalline substance, 0.8-1.2 part draw ratio is 14-16:
0.5-1.5 wollastonite raphioid fiber, the aqueous solution of 4.0-6.0 part mass fraction 25-35% sodium acid carbonate, 0.3-0.5 part golden red
Stone-type titanium dioxide, 0.2-0.4 part nano imvite, it is blended in stirring decatize reaction 45- in 150-170 DEG C of superheated steam reactor
60min, radiates 2-4h in 300-400 DEG C of vacuum microwave, is then dipped in the citric acid solution that 80-120 part mass fraction is 30%
Middle vacuum moisture absorption is processed, and is heated to 60-95 DEG C of ultrasonic wave dispersion 0.5-1.5h, is stirred for disperseing 2-4h, takes suspension after inhaling thoroughly,
With the deionized water of 60-100 part 3-5% containing mass fraction sodium tripolyphosphate dispersion liquid at 75-85 DEG C ultrasonication 25-
35min, takes upper strata suspension to filter through 100-200 mesh, distilled water washes clean, and cleaning and drying obtains strengthening age resister；
B) the enhancing age resister that step a) 8.0-12 part obtains, 6.0-10 part tdbppe phosphate, 1.0- are taken by mass fraction
3.0 parts of antimony oxides, 0.15-0.2 part 770 light stabilizer, 0.1-0.15 part dnp antioxidant, 0.4-0.6 part uv-327 ultraviolet
Light absorbers, the kr-212 coupling agent mixing of 5.0-10 part mass fraction 10-20% concentration, in mixer under the conditions of 80-90 DEG C
In flame-proof anti-aging agent is obtained with speed stirring reaction 45-60min of 250-350r/min, 50-70 DEG C of vacuum drying；
C) take, by mass fraction, the flame-proof anti-aging agent that step b) 8.0-12 part obtains, 3.0-6.0 part molecular weight 0.5-1's ten thousand is poly-
Ethylene glycol, 10-18 part ethylene glycol, 70-80 DEG C of high-speed stirred 0.5-1.5h, obtain feature ethylene glycol；
D) by mass fraction, 8.0 parts of terephthalic acid (TPA)s and 5.0 parts of ethylene glycol are first esterified, at class section of esterification
Or add 1.0-2.0 part in class kettle by c) prepared feature ethylene glycol, until esterification, polycondensation reaction complete to make fire-retardant
Anti-aging pet；
Or e) take, by mass fraction, the flame-proof anti-aging agent that step b) 8.0-12 part obtains, 2.0-5.0 part molecular weight 0.5-1's ten thousand
Polyethylene glycol, 80-120 part routine pet blended melting makes flame-proof anti-aging pet.
F) the flame-proof anti-aging pet obtaining step d) or step e) is cortex and conventional pet is sandwich layer, and melting is combined and makes skin
Core pattern lasting flame-proof anti-aging pet fiber.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108359083A (en) * | 2018-01-23 | 2018-08-03 | 浙江省现代纺织工业研究院 | A kind of preparation method of hybrid modification EG |
| CN108440743A (en) * | 2018-01-23 | 2018-08-24 | 浙江省现代纺织工业研究院 | A kind of preparation method of preposition modified EG |
| CN111019100A (en) * | 2018-10-10 | 2020-04-17 | 中国石油化工股份有限公司 | Montmorillonite-modified barrier polyester and preparation method thereof |
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| CN108359083A (en) * | 2018-01-23 | 2018-08-03 | 浙江省现代纺织工业研究院 | A kind of preparation method of hybrid modification EG |
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| CN111019100A (en) * | 2018-10-10 | 2020-04-17 | 中国石油化工股份有限公司 | Montmorillonite-modified barrier polyester and preparation method thereof |
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