CN106317390B - A kind of preparation method of moisture absorption antistatic polyester and fiber - Google Patents

A kind of preparation method of moisture absorption antistatic polyester and fiber Download PDF

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CN106317390B
CN106317390B CN201610791262.3A CN201610791262A CN106317390B CN 106317390 B CN106317390 B CN 106317390B CN 201610791262 A CN201610791262 A CN 201610791262A CN 106317390 B CN106317390 B CN 106317390B
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moisture absorption
mass fraction
polyester
suspended matter
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凌文嘉
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Southeast New material (Hangzhou) Co.,Ltd.
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Zhejiang Institute of Modern Textile Industry
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    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/66Polyesters containing oxygen in the form of ether groups
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/28Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
    • D01D5/30Conjugate filaments; Spinnerette packs therefor
    • D01D5/34Core-skin structure; Spinnerette packs therefor
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/09Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14Conjugated, 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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Abstract

The present invention relates to the preparation methods of a kind of moisture absorption antistatic polyester and fiber, belong to functional fiber preparing technical field, it is by talcum powder, sodium bicarbonate aqueous solution, concave convex rod is brilliant, conductive mica powder, it is dipped in sulfamic acid solution and disperses after halloysite nanotubes mixing progress decatize reaction, suspended matter is taken to perform etching, ultrasonication, after taking suspended matter filtration washing to dry again, with silane coupling agent alcoholic solution, diatomite, aluminium-doped zinc oxide, sodium bentonite, drying is mixed in antioxidant, the moisture absorption antistatic agent and ethylene glycol that will be obtained, polyethylene glycol stirs, it is added in class kettle, moisture absorption antistatic polyester is made;Using obtained moisture absorption antistatic polyester as cortex, using polyethylene terephthalate as sandwich layer, melting is combined moisture absorption anti-static polyester fiber.Highly hygroscopic material, conductive material are dispersed in the form of microfibril inside polyester by the present invention in preparation process, make have property through moisture absorption anti-static polyester fiber made of melting.

Description

A kind of preparation method of moisture absorption antistatic polyester and fiber
Technical field
The present invention relates to the preparation methods of a kind of moisture absorption antistatic polyester and fiber, belong to functional fiber technology of preparing neck Domain.
Background technology
Polyester fiber is with terephthalic acid (TPA) (PTA) or dimethyl terephthalate (DMT) (DMT) and ethylene glycol (EG) for raw material Through esterification or transesterification again through fiber-forming polymer-polyethylene terephthalate (PET) prepared by polycondensation reaction, through spinning Manufactured fiber, trade name terylene are the first big kinds of current synthetic fibers.Because fiber macromolecular chain rigidity is larger, Elasticity modulus is high, and fiber is unlikely to deform, therefore its fabric intensity is good, does not wrinkle after washing, can not press, it is strong very scrape, be washable easily dry, It is a kind of more satisfactory to take textile raw material.The official regain of polyester is 0.4%, be hair, flaxen fiber 1/30, polyester is fine The hygroscopicity of dimension is very poor, and resistivity is very high, and fabric resistor rate is up to 1015Ω cm or more are typically considered insulator.Moisture absorption The performance of antistatic fibre is primarily referred to as antistatic property, i.e., it quickly eliminates ability of electrostatic charge, standard state (RH65%, 20 DEG C) under, if resistivity≤109Ω cm belong to extraordinary antistatic fibre, if resistivity is 1010-1012Ω cm, then belong to Good antistatic fibre has a meaning of crucial importance in industry, the field of taking, and good hygroscopicity be more conducive to improve it is antistatic With the wearing comfort of fabric.
Diatomaceous density 1.9-2.3g/cm3, heap density 0.34-0.65g/cm3, specific surface area 40-65m/g, pore volume 0.45-0.98m, water absorption rate are 2-4 times of own vol, fusing point 1650C-1750, DEG C under an electron microscope it is observed that Special porous construction.Diatomaceous color is white, canescence, grey and terra brown etc., is had fine and smooth, loose, light, more Hole, water imbibition and the strong property of permeability.A small amount of diatomite is added in macromolecule polymer material can significantly improve material Adsorptivity and hygroscopicity, and can be improved product it is heat-resisting, heat preservation, it is anti-aging the effects that.
The basic structural unit of attapulgite is rodlike, needle-shaped, fibrous monocrystal, and abbreviation concave convex rod is brilliant, attapulgite The general < 50% of content of medium rod crystalline substance, concave convex rod crystalline substance are about 0.5-5 μm, and about 0.01-0.10 μm wide, surface is covered with concave-convex alternate Groove, 2-3 grades of Mohs' hardness are heated to 700-800 DEG C, 5 grades of hardness >, proportion 2.05-2.32.
Aluminium-doped zinc oxide, conductive mica powder addition have excellent anti-static function in PET.
Halloysite nanotubes are that a kind of kaolinic lamella crimps under natural endowment and forms natural many walls nanotube shape Material has typical many walls nanotube shape structure.Halloysite nanotubes are made of oxygen-octahedron, alumina octahedral, outer wall Containing certain silicone hydroxyl, combined in the form of the secondary bonds moral such as hydrogen bond and Van der Waals force between structural unit, to cation, polarity Molecule etc. has stronger adsorption capacity.Natural nano tubular structure and the property being easily dispersed so that halloysite nanotubes It is answered in polypropylene, epoxy resin, polyethylene, polyamide, polyester, rubber etc. as a kind of novel polymer reinforcing material With.
Bentonite is the aqueous clay pit based on montmorillonite, since it has special property, such as:Bloating tendency, bonding Property, adsorptivity, catalytic and cationic exchangeability etc., so being widely used in each industrial circle.Bentonitic interlayer sun from Subcategory determines that bentonitic type, interlayer cation claim sodium bentonite, sodium bentonite to have very strong moisture absorption when being Na+ Property and dilatancy, the water of adsorbable 8-15 times of own vol, volume expansion, to 30 times, there is stronger cation up to several times Exchange capacity and adsorption capacity have various gases, liquid, organic substance certain adsorption capacity, have higher plasticity and Stronger caking property, so the use value of sodium bentonite is very high.
Fiber worker has carried out a large amount of study on the modification for defect existing for polyester fiber for many years, to be made Polyester fiber with specific function.
Invention content
It is an object of the invention to overcome the shortcomings of the prior art, provide a kind of antistatic poly- with endogenous moisture absorption The preparation method of ester and fiber.
The preparation method of a kind of moisture absorption antistatic polyester of the present invention, using following steps:
A 0.2-0.4 parts of nanoscale talcum powders, the carbonic acid that 5.0-8.0 parts of mass fractions are 25-35%) are taken by mass fraction Hydrogen sodium water solution, 0.8-1.2 parts of characterization parameters are 0.5-5 μm a length of, width is 0.01-0.10 μm of concave convex rod crystalline substance, 1.0-2.0 parts of nanometers Grade conductive mica powder, 0.8-1.2 parts a diameter of 0.1-0.3 μm, the halloysite nanotubes that length is 0.5-5 μm, is blended in 140- Stirring decatize reacts 45-60min in 160 DEG C of superheated steam reaction kettles, radiates 1.5-2.5h in 350-450 DEG C of vacuum microwave, so It is dipped in vacuum moisture absorption in the sulfamic acid solution that 80-120 parts of mass fractions are 30% afterwards to handle, 60-95 DEG C is heated to after inhaling thoroughly Ultrasonic wave disperses 0.4-0.6h, is stirred for dispersion 1.5-2.5h, takes suspended matter;
B mass fraction) is pressed by step A) 2.0-4.0 part suspended matter microwave plasma etching processing 15-25min for obtaining, With the deionized water of the 60-100 parts of sodium tripolyphosphate dispersion liquids of 3-5% containing mass fraction at 70-90 DEG C ultrasonication 20- 40min, takes upper layer suspended matter to be filtered through 100-200 mesh, and distilled water washes clean, vacuum drying obtains anti-electrostatic nano material;
C) step B is taken by mass fraction) 12-18 parts of obtained anti-electrostatic nano materials, 8.0-15 parts of mass fractions are 20- 30% silane coupling agent alcoholic solution, 5.0-8.0 parts of microfine diatomaceous, 5.0-8.0 parts of aluminum-doped zinc oxide nanometer powders, 5.0- 8.0 parts of sodium bentonites, 1010 antioxidant of 0.1-0.3 parts mix, with 250-350r/min in mixing machine under the conditions of 50-70 DEG C Speed be stirred to react 45-60min, vacuum drying obtains moisture absorption antistatic agent under the conditions of 50-70 DEG C;
D) step C is taken by mass fraction) 8.0-18 parts of obtained moisture absorption antistatic agents, 12-20 parts of ethylene glycol, 2.0-5.0 The polyethylene glycol that part molecular weight is 0.5-1 ten thousand, high-speed stirred 0.5-1.5h under the conditions of 70-80 DEG C, it is right in esterifying kettle then to press The 20-35% of phthalic acid quality is added in class section of terephthalic acid (TPA) and ethylene glycol esterification or class kettle, Until esterification, polycondensation reaction are completed, moisture absorption antistatic polyester is made;
Or E) by mass fraction take step C) 6.0-15 parts of obtained moisture absorption antistatic agents, 2.0-5.0 parts of molecular weight are Polyethylene glycol and 90-110 part conventional polyethylene terephthalate blended melting of 0.5-1 ten thousand, is made moisture absorption antistatic polyester.
The preparation method of a kind of moisture absorption antistatic polyester of the present invention, using following steps:
A) 0.3 part of nanoscale talcum powder is taken by mass fraction, the sodium bicarbonate aqueous solution that 6.5 parts of mass fractions are 30%, 1.0 parts of characterization parameters are 2.5 μm a length of, width is 0.01-0.10 μm of concave convex rod crystalline substance, and 1.5 parts of nano-level conducting mica powders, 1.0 parts straight The halloysite nanotubes that diameter is 0.2 μm, length is 2.5 μm are blended in stirring decatize reaction in 150 DEG C of superheated steam reaction kettles 50min radiates 2h in 400 DEG C of vacuum microwaves, is then dipped in vacuum in the sulfamic acid solution that 100 parts of mass fractions are 30% and inhales Wet process is heated to 75 DEG C of ultrasonic wave dispersion 0.5h, is stirred for dispersion 2h, takes suspended matter after inhaling thoroughly;
B mass fraction) is pressed by step A) 3.0 parts of suspended matter microwave plasma etching processing 20min obtaining, contained with 80 parts The deionized water of 4% sodium tripolyphosphate dispersion liquid of mass fraction ultrasonication 30min at 80 DEG C takes upper layer suspended matter to pass through 150 mesh filter, and distilled water washes clean, vacuum drying obtains anti-electrostatic nano material;
C) take step B by mass fraction) 15 parts of obtained anti-electrostatic nano materials, 12 parts of mass fractions be 25% silane Coupling agent alcoholic solution, 6.5 parts of microfine diatomaceous, 6.5 parts of aluminum-doped zinc oxide nanometer powders, 6.5 parts of sodium bentonites, 0.2 part 1010 antioxidant mix, and 55min are stirred to react in mixing machine with the speed of 300r/min under the conditions of 60 DEG C, under the conditions of 60 DEG C Vacuum drying obtains moisture absorption antistatic agent;
D) step C is taken by mass fraction) 13 parts of obtained moisture absorption antistatic agents, 16 parts of ethylene glycol, 3.5 parts of molecular weight are 0.7 ten thousand polyethylene glycol, high-speed stirred 1h under the conditions of 75 DEG C, then press terephthalic acid (TPA) quality in esterifying kettle 25% are added To terephthalic acid (TPA) in class section of ethylene glycol esterification or class kettle, until esterification, polycondensation reaction are completed, it is made Moisture absorption antistatic polyester;
Or E) by mass fraction take step C) 10 parts of obtained moisture absorption antistatic agents, the poly- second that 3.5 parts of molecular weight are 0.7 ten thousand Glycol and 100 parts of conventional polyethylene terephthalate blended meltings, are made moisture absorption antistatic polyester.
The preparation method of a kind of moisture absorption anti-static polyester fiber of the present invention, using following steps:
A 0.2-0.4 parts of nanoscale talcum powders, the carbonic acid that 5.0-8.0 parts of mass fractions are 25-35%) are taken by mass fraction Hydrogen sodium water solution, 0.8-1.2 parts of characterization parameters are 0.5-5 μm a length of, width is 0.01-0.10 μm of concave convex rod crystalline substance, 1.0-2.0 parts of nanometers Grade conductive mica powder, 0.8-1.2 parts a diameter of 0.1-0.3 μm, the halloysite nanotubes that length is 0.5-5 μm, is blended in 140- Stirring decatize reacts 45-60min in 160 DEG C of superheated steam reaction kettles, radiates 1.5-2.5h in 350-450 DEG C of vacuum microwave, so It is dipped in vacuum moisture absorption in the sulfamic acid solution that 80-120 parts of mass fractions are 30% afterwards to handle, 60-95 DEG C is heated to after inhaling thoroughly Ultrasonic wave disperses 0.4-0.6h, is stirred for dispersion 1.5-2.5h, takes suspended matter;
B mass fraction) is pressed by step A) 2.0-4.0 part suspended matter microwave plasma etching processing 15-25min for obtaining, With the deionized water of the 60-100 parts of sodium tripolyphosphate dispersion liquids of 3-5% containing mass fraction at 70-90 DEG C ultrasonication 20- 40min, takes upper layer suspended matter to be filtered through 100-200 mesh, and distilled water washes clean, vacuum drying obtains anti-electrostatic nano material;
C) step B is taken by mass fraction) 12-18 parts of obtained anti-electrostatic nano materials, 8.0-15 parts of mass fractions are 20- 30% silane coupling agent alcoholic solution, 5.0-8.0 parts of microfine diatomaceous, 5.0-8.0 parts of aluminum-doped zinc oxide nanometer powders, 5.0- 8.0 parts of sodium bentonites, 1010 antioxidant of 0.1-0.3 parts mix, with 250-350r/min in mixing machine under the conditions of 50-70 DEG C Speed be stirred to react 45-60min, vacuum drying obtains moisture absorption antistatic agent under the conditions of 50-70 DEG C;
D) step C is taken by mass fraction) 8.0-18 parts of obtained moisture absorption antistatic agents, 12-20 parts of ethylene glycol, 2.0-5.0 The polyethylene glycol that part molecular weight is 0.5-1 ten thousand, high-speed stirred 0.5-1.5h under the conditions of 70-80 DEG C, it is right in esterifying kettle then to press The 20-35% of phthalic acid quality is added in class section of terephthalic acid (TPA) and ethylene glycol esterification or class kettle, Until esterification, polycondensation reaction are completed, moisture absorption antistatic polyester is made;
Or E) by mass fraction take step C) 6.0-15 parts of obtained moisture absorption antistatic agents, 2.0-5.0 parts of molecular weight are Polyethylene glycol and 90-110 part conventional polyethylene terephthalate blended melting of 0.5-1 ten thousand, is made moisture absorption antistatic polyester;
F) using step D) or step E) obtained moisture absorption antistatic polyester is cortex, with conventional polyethylene terephthalate For sandwich layer, melting is combined core-skin type moisture absorption anti-static polyester fiber.
Compared with prior art, the present invention applies halloysite nanotubes, diatomaceous superpower absorption in preparation process Performance and sodium bentonite, the absorption of conductive material and by absorbing synergic effect, while by highly hygroscopic material, conductive material with micro- Fibrinogen form is dispersed in inside polyester so that has particularity through core-skin type moisture absorption anti-static polyester fiber made of melting Energy.
Specific implementation mode
Below in conjunction with specific embodiment, the present invention will be described in detail:A kind of moisture absorption of the present invention is antistatic poly- The preparation method of ester, using following steps:
A 0.2-0.4 parts of nanoscale talcum powders, the carbonic acid that 5.0-8.0 parts of mass fractions are 25-35%) are taken by mass fraction Hydrogen sodium water solution, 0.8-1.2 parts of characterization parameters are 0.5-5 μm a length of, width is 0.01-0.10 μm of concave convex rod crystalline substance, 1.0-2.0 parts of nanometers Grade conductive mica powder, 0.8-1.2 parts a diameter of 0.1-0.3 μm, the halloysite nanotubes that length is 0.5-5 μm, is blended in 140- Stirring decatize reacts 45-60min in 160 DEG C of superheated steam reaction kettles, radiates 1.5-2.5h in 350-450 DEG C of vacuum microwave, so It is dipped in vacuum moisture absorption in the sulfamic acid solution that 80-120 parts of mass fractions are 30% afterwards to handle, 60-95 DEG C is heated to after inhaling thoroughly Ultrasonic wave disperses 0.4-0.6h, is stirred for dispersion 1.5-2.5h, takes suspended matter;
B mass fraction) is pressed by step A) 2.0-4.0 part suspended matter microwave plasma etching processing 15-25min for obtaining, With the deionized water of the 60-100 parts of sodium tripolyphosphate dispersion liquids of 3-5% containing mass fraction at 70-90 DEG C ultrasonication 20- 40min, takes upper layer suspended matter to be filtered through 100-200 mesh, and distilled water washes clean, vacuum drying obtains anti-electrostatic nano material;
C) step B is taken by mass fraction) 12-18 parts of obtained anti-electrostatic nano materials, 8.0-15 parts of mass fractions are 20- 30% silane coupling agent alcoholic solution, 5.0-8.0 parts of microfine diatomaceous, 5.0-8.0 parts of aluminum-doped zinc oxide nanometer powders, 5.0- 8.0 parts of sodium bentonites, 1010 antioxidant of 0.1-0.3 parts mix, with 250-350r/min in mixing machine under the conditions of 50-70 DEG C Speed be stirred to react 45-60min, vacuum drying obtains moisture absorption antistatic agent under the conditions of 50-70 DEG C;
D) step C is taken by mass fraction) 8.0-18 parts of obtained moisture absorption antistatic agents, 12-20 parts of ethylene glycol, 2-5 parts points Then the polyethylene glycol that son amount is 0.5-1 ten thousand, high-speed stirred 0.5-1.5h under the conditions of 70-80 DEG C are pressed in esterifying kettle to benzene two The 20-35% of formic acid quality is added in class section of terephthalic acid (TPA) and ethylene glycol esterification or class kettle, until Esterification, polycondensation reaction are completed, and moisture absorption antistatic polyester is made;
Or E) by mass fraction take step C) 6.0-15 parts of obtained moisture absorption antistatic agents, 2.0-5.0 parts of molecular weight are Polyethylene glycol and 90-110 part conventional polyethylene terephthalate blended melting of 0.5-1 ten thousand, is made moisture absorption antistatic polyester.
A kind of preparation method of moisture absorption anti-static polyester fiber, using following steps:
A 0.2-0.4 parts of nanoscale talcum powders, the carbonic acid that 5.0-8.0 parts of mass fractions are 25-35%) are taken by mass fraction Hydrogen sodium water solution, 0.8-1.2 parts of characterization parameters are 0.5-5 μm a length of, width is 0.01-0.10 μm of concave convex rod crystalline substance, 1.0-2.0 parts of nanometers Grade conductive mica powder, 0.8-1.2 parts a diameter of 0.1-0.3 μm, the halloysite nanotubes that length is 0.5-5 μm, is blended in 140- Stirring decatize reacts 45-60min in 160 DEG C of superheated steam reaction kettles, radiates 1.5-2.5h in 350-450 DEG C of vacuum microwave, so It is dipped in vacuum moisture absorption in the sulfamic acid solution that 80-120 parts of mass fractions are 30% afterwards to handle, 60-95 DEG C is heated to after inhaling thoroughly Ultrasonic wave disperses 0.4-0.6h, is stirred for dispersion 1.5-2.5h, takes suspended matter;
B mass fraction) is pressed by step A) 2.0-4.0 part suspended matter microwave plasma etching processing 15-25min for obtaining, With the deionized water of the 60-100 parts of sodium tripolyphosphate dispersion liquids of 3-5% containing mass fraction at 70-90 DEG C ultrasonication 20- 40min, takes upper layer suspended matter to be filtered through 100-200 mesh, and distilled water washes clean, vacuum drying obtains anti-electrostatic nano material;
C) step B is taken by mass fraction) 12-18 parts of obtained anti-electrostatic nano materials, 8.0-15 parts of mass fractions are 20- 30% silane coupling agent alcoholic solution, 5.0-8.0 parts of microfine diatomaceous, 5.0-8.0 parts of aluminum-doped zinc oxide nanometer powders, 5.0- 8.0 parts of sodium bentonites, 1010 antioxidant of 0.1-0.3 parts mix, with 250-350r/min in mixing machine under the conditions of 50-70 DEG C Speed be stirred to react 45-60min, vacuum drying obtains moisture absorption antistatic agent under the conditions of 50-70 DEG C;
D) step C is taken by mass fraction) 8.0-18 parts of obtained moisture absorption antistatic agents, 12-20 parts of ethylene glycol, 2.0-5.0 The polyethylene glycol that part molecular weight is 0.5-1 ten thousand, high-speed stirred 0.5-1.5h under the conditions of 70-80 DEG C, it is right in esterifying kettle then to press The 20-35% of phthalic acid quality is added in class section of terephthalic acid (TPA) and ethylene glycol esterification or class kettle, Until esterification, polycondensation reaction are completed, moisture absorption antistatic polyester is made;
Or E) by mass fraction take step C) 6.0-15 parts of obtained moisture absorption antistatic agents, 2.0-5.0 parts of molecular weight are Polyethylene glycol and 90-110 part conventional polyethylene terephthalate blended melting of 0.5-1 ten thousand, is made moisture absorption antistatic polyester;
F) using step D) or step E) obtained moisture absorption antistatic polyester is cortex, with conventional polyethylene terephthalate For sandwich layer, melting is combined core-skin type moisture absorption anti-static polyester fiber.
Embodiment 1:A kind of preparation method of moisture absorption antistatic polyester, using following steps:
A) 0.2 part of nanoscale talcum powder is taken by mass fraction, the sodium bicarbonate aqueous solution that 5.0 parts of mass fractions are 25%, 0.8 part of characterization parameter is 2.5 μm a length of, width is 0.01-0.10 μm of concave convex rod crystalline substance, and 1.0 parts of nano-level conducting mica powders, 0.8 part straight The halloysite nanotubes that diameter is 0.1 μm, length is 0.5 μm are blended in stirring decatize reaction in 140 DEG C of superheated steam reaction kettles 45min radiates 1.5h in 350 DEG C of vacuum microwaves, is then dipped in vacuum in the sulfamic acid solution that 80 parts of mass fractions are 30% Moisture absorption is handled, and 60 DEG C of ultrasonic wave dispersion 0.4h are heated to after inhaling thoroughly, dispersion 1.5h is stirred for, takes suspended matter;
B mass fraction) is pressed by step A) 2.0 parts of suspended matter microwave plasma etching processing 15min obtaining, contained with 60 parts The deionized water of 3% sodium tripolyphosphate dispersion liquid of mass fraction ultrasonication 20min at 70 DEG C takes upper layer suspended matter to pass through 100 mesh filter, and distilled water washes clean, vacuum drying obtains anti-electrostatic nano material;
C) take step B by mass fraction) 12 parts of obtained anti-electrostatic nano materials, 8.0 parts of mass fractions be 20% silicon Alkane coupling agent alcoholic solution, 5.0 parts of microfine diatomaceous, 5.0 parts of aluminum-doped zinc oxide nanometer powders, 5.0 parts of sodium bentonites, 0.1 1010 antioxidant of part mix, and 45min are stirred to react in mixing machine with the speed of 250r/min under the conditions of 50 DEG C, in 50 DEG C of conditions Lower vacuum drying obtains moisture absorption antistatic agent;
D) step C is taken by mass fraction) 8.0 parts of obtained moisture absorption antistatic agents, 12 parts of ethylene glycol, 2.0 parts of molecular weight are 0.5 ten thousand polyethylene glycol, high-speed stirred 0.5h under the conditions of 70 DEG C, then press terephthalic acid (TPA) quality in esterifying kettle 20% add Enter to terephthalic acid (TPA) in class section of ethylene glycol esterification or class kettle, until esterification, polycondensation reaction are completed, makes At moisture absorption antistatic polyester.
A kind of preparation method of moisture absorption anti-static polyester fiber, using following steps:
A) 0.2 part of nanoscale talcum powder is taken by mass fraction, the sodium bicarbonate aqueous solution that 5.0 parts of mass fractions are 25%, 0.8 part of characterization parameter is 2.5 μm a length of, width is 0.01-0.10 μm of concave convex rod crystalline substance, and 1.0 parts of nano-level conducting mica powders, 0.8 part straight The halloysite nanotubes that diameter is 0.1 μm, length is 0.5 μm are blended in stirring decatize reaction in 140 DEG C of superheated steam reaction kettles 45min radiates 1.5h in 350 DEG C of vacuum microwaves, is then dipped in vacuum in the sulfamic acid solution that 80 parts of mass fractions are 30% Moisture absorption is handled, and 60 DEG C of ultrasonic wave dispersion 0.4h are heated to after inhaling thoroughly, dispersion 1.5h is stirred for, takes suspended matter;
B mass fraction) is pressed by step A) 2.0 parts of suspended matter microwave plasma etching processing 15min obtaining, contained with 60 parts The deionized water of 3% sodium tripolyphosphate dispersion liquid of mass fraction ultrasonication 20min at 70 DEG C takes upper layer suspended matter to pass through 100 mesh filter, and distilled water washes clean, vacuum drying obtains anti-electrostatic nano material;
C) take step B by mass fraction) 12 parts of obtained anti-electrostatic nano materials, 8.0 parts of mass fractions be 20% silicon Alkane coupling agent alcoholic solution, 5.0 parts of microfine diatomaceous, 5.0 parts of aluminum-doped zinc oxide nanometer powders, 5.0 parts of sodium bentonites, 0.1 1010 antioxidant of part mix, and 45min are stirred to react in mixing machine with the speed of 250r/min under the conditions of 50 DEG C, in 50 DEG C of conditions Lower vacuum drying obtains moisture absorption antistatic agent;
D) step C is taken by mass fraction) 8.0 parts of obtained moisture absorption antistatic agents, 12 parts of ethylene glycol, 2.0 parts of molecular weight are 0.5 ten thousand polyethylene glycol, high-speed stirred 0.5h under the conditions of 70 DEG C, then press terephthalic acid (TPA) quality in esterifying kettle 20% add Enter to terephthalic acid (TPA) in class section of ethylene glycol esterification or class kettle, until esterification, polycondensation reaction are completed, makes At moisture absorption antistatic polyester;
E) using step D) obtained moisture absorption antistatic polyester is cortex, using conventional polyethylene terephthalate as sandwich layer, Melting is combined core-skin type moisture absorption anti-static polyester fiber.
Embodiment 2:A kind of preparation method of moisture absorption antistatic polyester, using following steps:
A) 0.3 part of nanoscale talcum powder is taken by mass fraction, the sodium bicarbonate aqueous solution that 6.5 parts of mass fractions are 30%, 1.0 parts of characterization parameters are 0.5-5 μm a length of, width is 0.01-0.10 μm of concave convex rod crystalline substance, 1.5 parts of nano-level conducting mica powders, 1.0 parts A diameter of 0.2 μm, the halloysite nanotubes that length is 2.5 μm are blended in stirring decatize reaction in 150 DEG C of superheated steam reaction kettles 50min radiates 2h in 400 DEG C of vacuum microwaves, is then dipped in vacuum in the sulfamic acid solution that 100 parts of mass fractions are 30% and inhales Wet process is heated to 75 DEG C of ultrasonic wave dispersion 0.5h, is stirred for dispersion 2h, takes suspended matter after inhaling thoroughly;
B mass fraction) is pressed by step A) 3.0 parts of suspended matter microwave plasma etching processing 20min obtaining, contained with 80 parts The deionized water of 4% sodium tripolyphosphate dispersion liquid of mass fraction ultrasonication 30min at 80 DEG C takes upper layer suspended matter to pass through 150 mesh filter, and distilled water washes clean, vacuum drying obtains anti-electrostatic nano material;
C) take step B by mass fraction) 15 parts of obtained anti-electrostatic nano materials, 12 parts of mass fractions be 25% silane Coupling agent alcoholic solution, 6.5 parts of microfine diatomaceous, 6.5 parts of aluminum-doped zinc oxide nanometer powders, 6.5 parts of sodium bentonites, 0.2 part 1010 antioxidant mix, and 55min are stirred to react in mixing machine with the speed of 300r/min under the conditions of 60 DEG C, under the conditions of 60 DEG C Vacuum drying obtains moisture absorption antistatic agent;
D) step C is taken by mass fraction) 10 parts of obtained moisture absorption antistatic agents, the poly- second two that 3.5 parts of molecular weight are 0.7 ten thousand Alcohol and 100 parts of conventional polyethylene terephthalate blended meltings, are made moisture absorption antistatic polyester.
A kind of preparation method of moisture absorption anti-static polyester fiber, using following steps:
A) 0.3 part of nanoscale talcum powder is taken by mass fraction, the sodium bicarbonate aqueous solution that 6.5 parts of mass fractions are 30%, 1.0 parts of characterization parameters are 0.5-5 μm a length of, width is 0.01-0.10 μm of concave convex rod crystalline substance, 1.5 parts of nano-level conducting mica powders, 1.0 parts A diameter of 0.2 μm, the halloysite nanotubes that length is 2.5 μm are blended in stirring decatize reaction in 150 DEG C of superheated steam reaction kettles 50min radiates 2h in 400 DEG C of vacuum microwaves, is then dipped in vacuum in the sulfamic acid solution that 100 parts of mass fractions are 30% and inhales Wet process is heated to 75 DEG C of ultrasonic wave dispersion 0.5h, is stirred for dispersion 2h, takes suspended matter after inhaling thoroughly;
B mass fraction) is pressed by step A) the 3.0 suspended matter microwave plasma etching processing 20min that obtain, contain matter with 80 parts The deionized water of amount 4% sodium tripolyphosphate dispersion liquid of score ultrasonication 30min at 80 DEG C, takes upper layer suspended matter through 150 Mesh filters, and distilled water washes clean, vacuum drying obtains anti-electrostatic nano material;
C) take step B by mass fraction) 15 parts of obtained anti-electrostatic nano materials, 12 parts of mass fractions be 25% silane Coupling agent alcoholic solution, 6.5 parts of microfine diatomaceous, 6.5 parts of aluminum-doped zinc oxide nanometer powders, 6.5 parts of sodium bentonites, 0.2 part 1010 antioxidant mix, and 55min are stirred to react in mixing machine with the speed of 300r/min under the conditions of 60 DEG C, under the conditions of 60 DEG C Vacuum drying obtains moisture absorption antistatic agent;
D) step C is taken by mass fraction) 10 parts of obtained moisture absorption antistatic agents, the poly- second two that 3.5 parts of molecular weight are 0.7 ten thousand Alcohol and 100 parts of conventional polyethylene terephthalate blended meltings, are made moisture absorption antistatic polyester;
E) using step D) obtained moisture absorption antistatic polyester is cortex, using conventional polyethylene terephthalate as sandwich layer, Melting is combined core-skin type moisture absorption anti-static polyester fiber.
Embodiment 3:A kind of preparation method of moisture absorption antistatic polyester, using following steps:
A) 0.4 part of nanoscale talcum powder is taken by mass fraction, the sodium bicarbonate aqueous solution that 8.0 parts of mass fractions are 35%, 1.2 parts of characterization parameters are 0.5-5 μm a length of, width is 0.01-0.10 μm of concave convex rod crystalline substance, 2.0 parts of nano-level conducting mica powders, 1.2 parts A diameter of 0.3 μm, the halloysite nanotubes that length is 5 μm are blended in stirring decatize reaction in 160 DEG C of superheated steam reaction kettles 60min radiates 2.5h in 450 DEG C of vacuum microwaves, is then dipped in vacuum in the sulfamic acid solution that 120 parts of mass fractions are 30% Moisture absorption is handled, and 95 DEG C of ultrasonic wave dispersion 0.6h are heated to after inhaling thoroughly, dispersion 2.5h is stirred for, takes suspended matter;
B mass fraction) is pressed by step A) 4.0 parts of suspended matter microwave plasma etching processing 25min obtaining, with 100 parts The deionized water of the 5% sodium tripolyphosphate dispersion liquid containing mass fraction ultrasonication 40min at 90 DEG C takes upper layer suspended matter to pass through 200 mesh filter, and distilled water washes clean, vacuum drying obtains anti-electrostatic nano material;
C) take step B by mass fraction) 18 parts of obtained anti-electrostatic nano materials, 15 parts of mass fractions be 30% silane Coupling agent alcoholic solution, 8.0 parts of microfine diatomaceous, 8.0 parts of aluminum-doped zinc oxide nanometer powders, 8.0 parts of sodium bentonites, 0.3 part 1010 antioxidant mix, and 60min are stirred to react in mixing machine with the speed of 350r/min under the conditions of 70 DEG C, under the conditions of 70 DEG C Vacuum drying obtains moisture absorption antistatic agent;
D) step C is taken by mass fraction) 18 parts of obtained moisture absorption antistatic agents, 20 parts of ethylene glycol, 5.0 parts of molecular weight are 1 Ten thousand polyethylene glycol, high-speed stirred 1.5h under the conditions of 80 DEG C, then press terephthalic acid (TPA) quality in esterifying kettle 35% are added To terephthalic acid (TPA) in class section of ethylene glycol esterification or class kettle, until esterification, polycondensation reaction are completed, it is made Moisture absorption antistatic polyester.
A kind of preparation method of moisture absorption anti-static polyester fiber, using following steps:
A) 0.4 part of nanoscale talcum powder is taken by mass fraction, the sodium bicarbonate aqueous solution that 8.0 parts of mass fractions are 35%, 1.2 parts of characterization parameters are 0.5-5 μm a length of, width is 0.01-0.10 μm of concave convex rod crystalline substance, 2.0 parts of nano-level conducting mica powders, 1.2 parts A diameter of 0.3 μm, the halloysite nanotubes that length is 5 μm are blended in stirring decatize reaction in 160 DEG C of superheated steam reaction kettles 60min radiates 2.5h in 450 DEG C of vacuum microwaves, is then dipped in vacuum in the sulfamic acid solution that 120 parts of mass fractions are 30% Moisture absorption is handled, and 95 DEG C of ultrasonic wave dispersion 0.6h are heated to after inhaling thoroughly, dispersion 2.5h is stirred for, takes suspended matter;
B mass fraction) is pressed by step A) 4.0 parts of suspended matter microwave plasma etching processing 25min obtaining, with 100 parts The deionized water of the 5% sodium tripolyphosphate dispersion liquid containing mass fraction ultrasonication 40min at 90 DEG C takes upper layer suspended matter to pass through 200 mesh filter, and distilled water washes clean, vacuum drying obtains anti-electrostatic nano material;
C) take step B by mass fraction) 18 parts of obtained anti-electrostatic nano materials, 15 parts of mass fractions be 30% silane Coupling agent alcoholic solution, 8.0 parts of microfine diatomaceous, 8.0 parts of aluminum-doped zinc oxide nanometer powders, 8.0 parts of sodium bentonites, 0.3 part 1010 antioxidant mix, and 60min are stirred to react in mixing machine with the speed of 350r/min under the conditions of 70 DEG C, under the conditions of 70 DEG C Vacuum drying obtains moisture absorption antistatic agent;
D) step C is taken by mass fraction) 18 parts of obtained moisture absorption antistatic agents, 20 parts of ethylene glycol, 5.0 parts of molecular weight are 1 Ten thousand polyethylene glycol, high-speed stirred 1.5h under the conditions of 80 DEG C, then press terephthalic acid (TPA) quality in esterifying kettle 35% are added To terephthalic acid (TPA) in class section of ethylene glycol esterification or class kettle, until esterification, polycondensation reaction are completed, it is made Moisture absorption antistatic polyester;
E) using step D) obtained moisture absorption antistatic polyester is cortex, using conventional polyethylene terephthalate as sandwich layer, Melting is combined core-skin type moisture absorption anti-static polyester fiber.
Embodiment of the present invention is not limited to embodiment described above, by aforementioned disclosed numberical range, just Arbitrary replacement is carried out in specific embodiment, and so as to obtain numerous embodiment, this is not enumerated.

Claims (3)

1. a kind of preparation method of moisture absorption antistatic polyester, it is characterised in that the preparation method uses following steps:
A 0.2-0.4 parts of nanoscale talcum powders, the sodium bicarbonate that 5.0-8.0 parts of mass fractions are 25-35%) are taken by mass fraction Aqueous solution, 0.8-1.2 parts of characterization parameters are 0.5-5 μm a length of, width is 0.01-0.10 μm of concave convex rod crystalline substance, and 1.0-2.0 parts of nanoscales are led Electric mica powder, 0.8-1.2 parts a diameter of 0.1-0.3 μm, the halloysite nanotubes that length is 0.5-5 μm, is blended in 140-160 DEG C Stirring decatize reacts 45-60min in superheated steam reaction kettle, radiates 1.5-2.5h in 350-450 DEG C of vacuum microwave, is then dipped in Vacuum moisture absorption is handled in the sulfamic acid solution that 80-120 parts of mass fractions are 30%, and 60-95 DEG C of ultrasonic wave is heated to after inhaling thoroughly Disperse 0.4-0.6h, is stirred for dispersion 1.5-2.5h, takes suspended matter;
B mass fraction) is pressed by step A) 2.0-4.0 part suspended matter microwave plasma etching processing 15-25min for obtaining, use 60- The deionized water of 100 parts of sodium tripolyphosphate dispersion liquids of 3-5% containing mass fraction ultrasonication 20-40min at 70-90 DEG C, Upper layer suspended matter is taken to be filtered through 100-200 mesh, distilled water washes clean, vacuum drying obtains anti-electrostatic nano material;
C) step B is taken by mass fraction) 12-18 parts of obtained anti-electrostatic nano materials, 8.0-15 parts of mass fractions are 20-30% Silane coupling agent alcoholic solution, 5.0-8.0 parts of microfine diatomaceous, 5.0-8.0 parts of aluminum-doped zinc oxide nanometer powders, 5.0-8.0 Part sodium bentonite, 1010 antioxidant of 0.1-0.3 parts mix, with 250-350r/min's in mixing machine under the conditions of 50-70 DEG C Speed is stirred to react 45-60min, and vacuum drying obtains moisture absorption antistatic agent under the conditions of 50-70 DEG C;
D) step C is taken by mass fraction) 8.0-18 parts of obtained moisture absorption antistatic agents, 12-20 parts of ethylene glycol, 2.0-5.0 parts points Then the polyethylene glycol that son amount is 0.5-1 ten thousand, high-speed stirred 0.5-1.5h under the conditions of 70-80 DEG C are pressed in esterifying kettle to benzene two The 20-35% of formic acid quality is added in terephthalic acid (TPA) and the class kettle of ethylene glycol esterification, up to esterification, polycondensation are anti- It should complete, moisture absorption antistatic polyester is made;
Or E) by mass fraction take step C) 6.0-15 parts of obtained moisture absorption antistatic agents, 2.0-5.0 parts of molecular weight are 0.5-1 ten thousand Polyethylene glycol and 90-110 parts of conventional polyethylene terephthalate blended meltings, moisture absorption antistatic polyester is made.
2. a kind of preparation method of moisture absorption antistatic polyester, it is characterised in that the preparation method uses following steps:
A) 0.3 part of nanoscale talcum powder is taken by mass fraction, the sodium bicarbonate aqueous solution that 6.5 parts of mass fractions are 30%, 1.0 parts Characterization parameter is 2.5 μm a length of, width is 0.01-0.10 μm of concave convex rod crystalline substance, and 1.5 parts of nano-level conducting mica powders, 1.0 parts a diameter of 0.2 μm, the halloysite nanotubes that length is 2.5 μm are blended in stirring decatize reaction 50min in 150 DEG C of superheated steam reaction kettles, 2h is radiated in 400 DEG C of vacuum microwaves, is then dipped in the sulfamic acid solution that 100 parts of mass fractions are 30% at vacuum moisture absorption Reason is heated to 75 DEG C of ultrasonic wave dispersion 0.5h, is stirred for dispersion 2h, takes suspended matter after inhaling thoroughly;
B mass fraction) is pressed by step A) 3.0 parts of suspended matter microwave plasma etching processing 20min obtaining, contain quality with 80 parts The deionized water of 4% sodium tripolyphosphate dispersion liquid of score ultrasonication 30min at 80 DEG C, takes upper layer suspended matter through 150 mesh Filtering, distilled water washes clean, vacuum drying obtain anti-electrostatic nano material;
C) take step B by mass fraction) 15 parts of obtained anti-electrostatic nano materials, 12 parts of mass fractions be 25% it is silane coupled Agent alcoholic solution, 6.5 parts of microfine diatomaceous, 6.5 parts of aluminum-doped zinc oxide nanometer powders, 6.5 parts of sodium bentonites, 0.2 part 1010 Antioxidant mixes, and is stirred to react 55min in mixing machine with the speed of 300r/min under the conditions of 60 DEG C, vacuum under the conditions of 60 DEG C Drying obtains moisture absorption antistatic agent;
D) step C is taken by mass fraction) 13 parts of obtained moisture absorption antistatic agents, 16 parts of ethylene glycol, 3.5 parts of molecular weight are 0.7 ten thousand Polyethylene glycol, then high-speed stirred 1h under the conditions of 75 DEG C is added to pair by 25% of terephthalic acid (TPA) quality in esterifying kettle With in the class kettle of ethylene glycol esterification, until esterification, polycondensation reaction are completed, it is antistatic poly- that moisture absorption is made in phthalic acid Ester;
Or E) by mass fraction take step C) 10 parts of obtained moisture absorption antistatic agents, the polyethylene glycol that 3.5 parts of molecular weight are 0.7 ten thousand With 100 parts of conventional polyethylene terephthalate blended meltings, moisture absorption antistatic polyester is made.
3. a kind of preparation method of moisture absorption anti-static polyester fiber, it is characterised in that the preparation method uses following steps:
A 0.2-0.4 parts of nanoscale talcum powders, the sodium bicarbonate that 5.0-8.0 parts of mass fractions are 25-35%) are taken by mass fraction Aqueous solution, 0.8-1.2 parts of characterization parameters are 0.5-5 μm a length of, width is 0.01-0.10 μm of concave convex rod crystalline substance, and 1.0-2.0 parts of nanoscales are led Electric mica powder, 0.8-1.2 parts a diameter of 0.1-0.3 μm, the halloysite nanotubes that length is 0.5-5 μm, is blended in 140-160 DEG C Stirring decatize reacts 45-60min in superheated steam reaction kettle, radiates 1.5-2.5h in 350-450 DEG C of vacuum microwave, is then dipped in Vacuum moisture absorption is handled in the sulfamic acid solution that 80-120 parts of mass fractions are 30%, and 60-95 DEG C of ultrasonic wave is heated to after inhaling thoroughly Disperse 0.4-0.6h, is stirred for dispersion 1.5-2.5h, takes suspended matter;
B mass fraction) is pressed by step A) 2.0-4.0 part suspended matter microwave plasma etching processing 15-25min for obtaining, use 60- The deionized water of 100 parts of sodium tripolyphosphate dispersion liquids of 3-5% containing mass fraction ultrasonication 20-40min at 70-90 DEG C, Upper layer suspended matter is taken to be filtered through 100-200 mesh, distilled water washes clean, vacuum drying obtains anti-electrostatic nano material;
C) step B is taken by mass fraction) 12-18 parts of obtained anti-electrostatic nano materials, 8.0-15 parts of mass fractions are 20-30% Silane coupling agent alcoholic solution, 5.0-8.0 parts of microfine diatomaceous, 5.0-8.0 parts of aluminum-doped zinc oxide nanometer powders, 5.0-8.0 Part sodium bentonite, 1010 antioxidant of 0.1-0.3 parts mix, with 250-350r/min's in mixing machine under the conditions of 50-70 DEG C Speed is stirred to react 45-60min, and vacuum drying obtains moisture absorption antistatic agent under the conditions of 50-70 DEG C;
D) step C is taken by mass fraction) 8.0-18 parts of obtained moisture absorption antistatic agents, 12-20 parts of ethylene glycol, 2.0-5.0 parts points Then the polyethylene glycol that son amount is 0.5-1 ten thousand, high-speed stirred 0.5-1.5h under the conditions of 70-80 DEG C are pressed in esterifying kettle to benzene two The 20-35% of formic acid quality is added in terephthalic acid (TPA) and the class kettle of ethylene glycol esterification, up to esterification, polycondensation are anti- It should complete, moisture absorption antistatic polyester is made;
Or E) by mass fraction take step C) 6.0-15 parts of obtained moisture absorption antistatic agents, 2.0-5.0 parts of molecular weight are 0.5-1 ten thousand Polyethylene glycol and 90-110 parts of conventional polyethylene terephthalate blended meltings, moisture absorption antistatic polyester is made;
F) using step D) or step E) obtained moisture absorption antistatic polyester is cortex, using conventional polyethylene terephthalate as core Layer, melting are combined core-skin type moisture absorption anti-static polyester fiber.
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