CN102978731B - Method for manufacturing polyvinyl acetal conductive fibers - Google Patents
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- CN102978731B CN102978731B CN201210489353.3A CN201210489353A CN102978731B CN 102978731 B CN102978731 B CN 102978731B CN 201210489353 A CN201210489353 A CN 201210489353A CN 102978731 B CN102978731 B CN 102978731B
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- 239000000835 fiber Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 36
- 229920002554 vinyl polymer Polymers 0.000 title claims abstract description 26
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 125000002777 acetyl group Chemical class [H]C([H])([H])C(*)=O 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 55
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 55
- 238000009987 spinning Methods 0.000 claims abstract description 38
- 238000001914 filtration Methods 0.000 claims abstract description 33
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 20
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000005516 engineering process Methods 0.000 claims abstract description 13
- 239000006229 carbon black Substances 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 11
- 239000011787 zinc oxide Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000013078 crystal Substances 0.000 claims description 54
- 239000000203 mixture Substances 0.000 claims description 32
- 238000003756 stirring Methods 0.000 claims description 24
- 238000012512 characterization method Methods 0.000 claims description 16
- 239000007822 coupling agent Substances 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 11
- 235000019241 carbon black Nutrition 0.000 claims description 10
- 239000006185 dispersion Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 8
- 238000006359 acetalization reaction Methods 0.000 claims description 8
- 150000004645 aluminates Chemical class 0.000 claims description 8
- 229910052787 antimony Inorganic materials 0.000 claims description 8
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 8
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 8
- 235000013539 calcium stearate Nutrition 0.000 claims description 8
- 239000008116 calcium stearate Substances 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000010030 laminating Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 8
- 239000000725 suspension Substances 0.000 claims description 8
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 8
- 229910001887 tin oxide Inorganic materials 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000004020 conductor Substances 0.000 abstract description 6
- 239000002131 composite material Substances 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 2
- 229920000742 Cotton Polymers 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 229920002994 synthetic fiber Polymers 0.000 description 3
- 239000012209 synthetic fiber Substances 0.000 description 3
- 229920002978 Vinylon Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 210000002950 fibroblast Anatomy 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
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Abstract
The invention relates to a method for manufacturing polyvinyl acetal conductive fibers. The method comprises the following steps of: adding conducting materials including ATO conductive powder, superconducting carbon black, zinc oxide whiskers, potassium titanate whiskers and the like into a fiber-grade polyvinyl alcohol spinning solution, and mixing, filtering and defoaming to prepare a conductive polyvinyl alcohol spinning solution; and ensuring that one part of the fibers becomes composite polyvinyl acetal conductive fibers containing conductive substances through a composite spinning technology. The polyvinyl acetal conductive fibers have low resistivity, high strength, durability and conductivity even the humidity is low.
Description
Technical field
The present invention relates to a kind of manufacture method of Pioloform, polyvinyl acetal conductive fiber, comprise fibre-grade polyvinyl alcohol (PVA), ATO conducting powder, superconductive carbon black, ZnOw (ZnO), the manufacture method of the conductive fibers such as electric conductivity potassium titanate crystal whisker (PTW), belongs to chemical fibre manufacturing technology.
Background technology
The fiber that the polyvinyl alcohol of take makes as raw material spinning, by this fiber, through the resulting vinylon of formaldehyde treated, China claims polyvinyl, claims in the world vinylon.The character of polyvinyl is quite similar to cotton, has the title of synthetic cotton, and intensity and ABRASION RESISTANCE are better than cotton; Polyvinyl long filament is again as silk, and hygroscopicity is better, and under standard state, regain is 4.5～5%, in synthetic fiber, comes out at the top; Proportion (1.26～1.30) is less than cotton, and pyroconductivity is lower, and warmth retention property is better; Corrosion resistance, be difficult for mould moth; Polyvinyl has good hygroscopicity, gas permeability, flexibility, comfortable and easy to wear; Be widely used in that clothes, family spin, the field such as non-weaving cloth.
Conductive fiber typically refers to (20 ℃, 65% relative humidity), the fiber than resistance below 107 Ω cm under standard state, this fibrid has good electric conductivity and durability, therefore particularly under low humidity, still there is good durable electric conductivity, in the field such as industrial, civilian, have very large purposes.Take fibroblast high molecular polymer as matrix, with coating or complex method, add the conductive fiber of conductive materials, by composite spinning technology, make a part for fiber contain conductive materials, make like this fiber when thering is conductive characteristic, have again the processing characteristics of common synthetic fiber excellence concurrently, become the functional fiber with spinnability.
Whisker is the diameter very little (0.1～10um), atomic arrangement high-sequential, the intensity that form with the monocrystalline form growth theoretical value that approaches perfect crystal, the fibrous material that has certain draw ratio (5～1000); In high molecular polymer, add a small amount of whisker, as ZnOw, potassium titanate crystal whisker etc., just can not only strengthen but also toughness reinforcing, also can improve other performances such as conduction.
In the whisker of numerous kinds, four acicular type zinc oxide crystal whisker (ZnO) is given its outstanding electric conductivity with solid four acicular textures of its uniqueness; ZnO itself is N-shaped semiconductor, and four-feet needle-shaped whisker three-dimensional extension structure, while being dispersed in matrix, being close to each needle-like position and mutually overlapping formation conductive path in addition, electric charge is conducted, thereby give material electric conductivity.Electric conductivity potassium titanate crystal whisker (PTW) is a kind of staple fibre compound of novel needle-like, and because its size is tiny, perfect crystalline, has the good physical and mechanical propertiess such as conduction.
Scientific worker be take polyester material as matrix for many years, to add conductive materials mode, develops macromolecular material conductive fiber; But the electric conductivity of this class conductive fiber, fibre strength are all not so good, are in use very limited.
Summary of the invention
The object of the invention is to overcome the deficiency that prior art exists, a kind of have good electric conductivity and durability are provided, particularly under low humidity, still there is the manufacture method of the good durable Pioloform, polyvinyl acetal conductive fiber from natural disposition, electric conductivity.
The object of the invention is to complete by following technical solution, the manufacture method of described Pioloform, polyvinyl acetal conductive fiber, this manufacture method adopts following steps:
A) by mass fraction, getting 12-18 part characterization parameter diameter is 0.2-1um, the four acicular type zinc oxide crystal whisker that length is 5-15um; 3-8 part characterization parameter diameter is 0.2-0.6um, the electric conductivity potassium titanate crystal whisker that length is 5-12um; After above-mentioned material is mixed, at 300-400 ℃ of vacuum kiln roasting 4-6h; Cooling rear by calgon dispersed with stirring in absolute ethyl alcohol, at atmospheric plasma, process 10-20min; Then, cleaning 25-35min loose with the 60-70 ℃ of deionized water for ultrasonic wavelength-division containing calcium stearate dispersion, gets solution upper strata suspension whisker and removes after filtration the above particle of 16um, and repeat 3-5 time until filtering; After filtering, at vacuum drying oven, dry, obtain modified crystal whiskers mixture;
B) by mass fraction, get steps A) modified crystal whiskers mixture 4-8 part of obtaining, antimony doped tin oxide conducting powder 2-4 part, superconductive carbon black 5-9 part, titanate coupling agent 0.1-0.2 part, aluminate coupling agent 0.1-0.2 part, Tissuemat E 1.5-2.0 part, under 60-70 ℃ of condition, turn/min of mixer 250-400 stirs 45-60min; Obtain modified crystal whiskers conduction blend;
C) by mass fraction, be under the condition that exists at micro-calgon of the modified crystal whiskers conduction blend of 30-45 part, add polyvinyl alcohol spin dope 80-120 part, at 90-95 ℃ of temperature, middling speed stirs 45-60min, obtains conductive polyvinyl alcohol spinning solution;
D) by step C) after conductive polyvinyl alcohol spinning solution mixing under 90-95 ℃ of constant temperature of obtaining, filtration, deaeration, conductive polyvinyl alcohol spinning solution and the polyvinyl alcohol spin dope of 25-35 ﹕ 75-65 in mass ratio, through wet method or the spinning of dry laminating spining technology, acetalization, makes a kind of Pioloform, polyvinyl acetal conductive fiber that conductive polyvinyl alcohol is cortex of take.
Preferable production process of the present invention, comprises the steps:
A) by mass fraction, getting 15 parts of characterization parameter diameters is 0.2-1um, the four acicular type zinc oxide crystal whisker that length is 5-15um; 5 parts of characterization parameter diameters are 0.2-0.6um, the electric conductivity potassium titanate crystal whisker that length is 5-12um; After above-mentioned material is mixed, at 350 ℃ of vacuum kiln roasting 5h; Cooling rear by calgon dispersed with stirring in absolute ethyl alcohol, at atmospheric plasma, process 15min; Then, cleaning 30min loose with 65 ℃ of deionized water for ultrasonic wavelength-divisions containing calcium stearate dispersion, gets solution upper strata suspension whisker and removes after filtration the above particle of 16um, and repeat 3-5 time until filtering; After filtering, at vacuum drying oven, dry, obtain modified crystal whiskers mixture;
B) by mass fraction, get steps A) 6 parts, the modified crystal whiskers mixture that obtains, 3 parts of antimony doped tin oxide conducting powder, 7 parts of superconduction superconductive carbon blacks, 0.15 part of titanate coupling agent, 0.15 part of aluminate coupling agent, 1.7 parts of Tissuemat Es, under 65 ℃ of conditions, turn/min of mixer 300 stirs 50min; Obtain modified crystal whiskers conduction blend;
C) by mass fraction, be under the condition that exists at micro-calgon of the modified crystal whiskers conduction blend of 40 parts, add 100 parts of polyvinyl alcohol spin dopes, at 92 ℃ of temperature, middling speed stirs 50min, obtains conductive polyvinyl alcohol spinning solution;
D) by step C) after conductive polyvinyl alcohol spinning solution mixing under 92 ℃ of constant temperature of obtaining, filtration, deaeration, conductive polyvinyl alcohol spinning solution and the polyvinyl alcohol spin dope of 30 ﹕ 70 in mass ratio, through wet method or the spinning of dry laminating spining technology, acetalization, makes a kind of Pioloform, polyvinyl acetal conductive fiber that conductive polyvinyl alcohol is cortex of take.
The present invention adds and comprises ATO conducting powder in fibre-grade polyvinyl alcohol, superconductive carbon black, ZnOw, the conductive materials such as potassium titanate crystal whisker, make the cortex of fiber contain conductive materials by composite spinning technology, make like this fiber when having conductive characteristic, have again the processing characteristics of common synthetic fiber excellence concurrently, become the conductive fiber with spinnability, thereby obtain low-resistivity, the conductive polyvinyl alcohol acetal fibre of high fracture strength; This fibrid has good electric conductivity and durability, particularly under low humidity, still has good durablely from natural disposition electric conductivity, therefore in the field such as industrial, civilian, has very large purposes.
The specific embodiment
Below in conjunction with specific embodiment, the present invention will be described in detail: the manufacture method of Pioloform, polyvinyl acetal conductive fiber of the present invention, and this manufacture method adopts following steps:
A) by mass fraction, getting 12-18 part characterization parameter diameter is 0.2-1um, the four acicular type zinc oxide crystal whisker that length is 5-15um; 3-8 part characterization parameter diameter is 0.2-0.6um, the electric conductivity potassium titanate crystal whisker that length is 5-12um; After above-mentioned material is mixed, at 300-400 ℃ of vacuum kiln roasting 4-6h; Cooling rear by calgon dispersed with stirring in absolute ethyl alcohol, at atmospheric plasma, process 10-20min; Then, cleaning 25-35min loose with the 60-70 ℃ of deionized water for ultrasonic wavelength-division containing calcium stearate dispersion, gets solution upper strata suspension whisker and removes after filtration the above particle of 16um, and repeat 3-5 time until filtering; After filtering, at vacuum drying oven, dry, obtain modified crystal whiskers mixture;
B) by mass fraction, get steps A) modified crystal whiskers mixture 4-8 part of obtaining, 24 parts of antimony doped tin oxide conducting powder, superconduction superconductive carbon black 5-9 part, titanate coupling agent 0.1-0.2 part, aluminate coupling agent 0.1-0.2 part, Tissuemat E 1.5-2.0 part, under 60-70 ℃ of condition, turn/min of mixer 250-400 stirs 45-60min; Obtain modified crystal whiskers conduction blend;
C) by mass fraction, be under the condition that exists at micro-calgon of the modified crystal whiskers conduction blend of 30-45 part, add polyvinyl alcohol spin dope 80-120 part, at 90-95 ℃ of temperature, middling speed stirs 45-60min, obtains conductive polyvinyl alcohol spinning solution;
D) by step C) after conductive polyvinyl alcohol spinning solution mixing under 90-95 ℃ of constant temperature of obtaining, filtration, deaeration, conductive polyvinyl alcohol spinning solution and the polyvinyl alcohol spin dope of 25-35 ﹕ 75-65 in mass ratio, through wet method or the spinning of dry laminating spining technology, acetalization, makes a kind of Pioloform, polyvinyl acetal conductive fiber that conductive polyvinyl alcohol is cortex of take.
Embodiments of the invention can be selected arbitrarily in each number range by various parameters by technique scheme; thereby obtain numerous specific embodiment; therefore; protection scope of the present invention is not limited to following embodiment; and for the embodiment of following discloses; numerical value by various parameters is replaced, and can obtain numerous embodiment equally.
Embodiment 1:
The manufacture method of Pioloform, polyvinyl acetal conductive fiber of the present invention, it comprises the steps:
A) by mass fraction, getting 15 parts of characterization parameter diameters is 0.2-1um, the four acicular type zinc oxide crystal whisker that length is 5-15um; 5 parts of characterization parameter diameters are 0.2-0.6um, the electric conductivity potassium titanate crystal whisker that length is 5-12um; After above-mentioned material is mixed, at 350 ℃ of vacuum kiln roasting 5h; Cooling rear by calgon dispersed with stirring in absolute ethyl alcohol, at atmospheric plasma, process 15min; Then, cleaning 30min loose with 65 ℃ of deionized water for ultrasonic wavelength-divisions containing calcium stearate dispersion, gets solution upper strata suspension whisker and removes after filtration the above particle of 16um, and repeat 3-5 time until filtering; After filtering, at vacuum drying oven, dry, obtain modified crystal whiskers mixture;
B) by mass fraction, get steps A) 6 parts, the modified crystal whiskers mixture that obtains, 3 parts of antimony doped tin oxide conducting powder, 7 parts of superconduction superconductive carbon blacks, 0.15 part of titanate coupling agent, 0.15 part of aluminate coupling agent, 1.7 parts of Tissuemat Es, under 65 ℃ of conditions, turn/min of mixer 300 stirs 50min; Obtain modified crystal whiskers conduction blend;
C) by mass fraction, be under the condition that exists at micro-calgon of the modified crystal whiskers conduction blend of 40 parts, add 100 parts of polyvinyl alcohol spin dopes, at 92 ℃ of temperature, middling speed stirs 50min, obtains conductive polyvinyl alcohol spinning solution;
D) by step C) after conductive polyvinyl alcohol spinning solution mixing under 92 ℃ of constant temperature of obtaining, filtration, deaeration, conductive polyvinyl alcohol spinning solution and the polyvinyl alcohol spin dope of 30 ﹕ 70 in mass ratio, through wet method or the spinning of dry laminating spining technology, acetalization, makes a kind of Pioloform, polyvinyl acetal conductive fiber that conductive polyvinyl alcohol is cortex of take.
Embodiment 2:
The manufacture method of Pioloform, polyvinyl acetal conductive fiber of the present invention, this manufacture method adopts following steps:
A) by mass fraction, getting 12 parts of characterization parameter diameters is 0.2-1um, the four acicular type zinc oxide crystal whisker that length is 5-15um; 3 parts of characterization parameter diameters are 0.2-0.6um, the electric conductivity potassium titanate crystal whisker that length is 5-12um; After above-mentioned material is mixed, at 300 ℃ of vacuum kiln roasting 4h; Cooling rear by calgon dispersed with stirring in absolute ethyl alcohol, at atmospheric plasma, process 10min; Then, cleaning 25-35min loose with 60 ℃ of deionized water for ultrasonic wavelength-divisions containing calcium stearate dispersion, gets solution upper strata suspension whisker and removes after filtration the above particle of 16um, and repeat 3 times until filtering; After filtering, at vacuum drying oven, dry, obtain modified crystal whiskers mixture;
B) by mass fraction, get steps A) 4 parts, the modified crystal whiskers mixture that obtains, 2 parts of antimony doped tin oxide conducting powder, 5 parts of superconduction superconductive carbon blacks, 0.1 part of titanate coupling agent, 0.1 part of aluminate coupling agent, 1.5 parts of Tissuemat Es, under 60 ℃ of conditions, turn/min of mixer 250 stirs 45min; Obtain modified crystal whiskers conduction blend;
C) by mass fraction, be under the condition that exists at micro-calgon of the modified crystal whiskers conduction blend of 30 parts, add 80 parts of polyvinyl alcohol spin dopes, at 90 ℃ of temperature, middling speed stirs 45min, obtains conductive polyvinyl alcohol spinning solution;
D) by step C) after conductive polyvinyl alcohol spinning solution mixing under 90 ℃ of constant temperature of obtaining, filtration, deaeration, conductive polyvinyl alcohol spinning solution and the polyvinyl alcohol spin dope of 25 ﹕ 75 in mass ratio, through wet method or the spinning of dry laminating spining technology, acetalization, makes a kind of Pioloform, polyvinyl acetal conductive fiber that conductive polyvinyl alcohol is cortex of take.
Embodiment 3:
The manufacture method of Pioloform, polyvinyl acetal conductive fiber of the present invention, this manufacture method adopts following steps:
A) by mass fraction, getting 18 parts of characterization parameter diameters is 0.2-1um, the four acicular type zinc oxide crystal whisker that length is 5-15um; 8 parts of characterization parameter diameters are 0.2-0.6um, the electric conductivity potassium titanate crystal whisker that length is 5-12um; After above-mentioned material is mixed, at 400 ℃ of vacuum kiln roasting 6h; Cooling rear by calgon dispersed with stirring in absolute ethyl alcohol, at atmospheric plasma, process 20min; Then, cleaning 35min loose with 70 ℃ of deionized water for ultrasonic wavelength-divisions containing calcium stearate dispersion, gets solution upper strata suspension whisker and removes after filtration the above particle of 16um, and repeat 5 times until filtering; After filtering, at vacuum drying oven, dry, obtain modified crystal whiskers mixture;
B) by mass fraction, get steps A) 8 parts, the modified crystal whiskers mixture that obtains, 4 parts of antimony doped tin oxide conducting powder, 9 parts of superconduction superconductive carbon blacks, 0.2 part of titanate coupling agent, 0.2 part of aluminate coupling agent, 2.0 parts of Tissuemat Es, under 70 ℃ of conditions, turn/min of mixer 400 stirs 60min; Obtain modified crystal whiskers conduction blend;
C) by mass fraction, be under the condition that exists at micro-calgon of the modified crystal whiskers conduction blend of 45 parts, add 120 parts of polyvinyl alcohol spin dopes, at 95 ℃ of temperature, middling speed stirs 60min, obtains conductive polyvinyl alcohol spinning solution;
D) by step C) after conductive polyvinyl alcohol spinning solution mixing under 95 ℃ of constant temperature of obtaining, filtration, deaeration, conductive polyvinyl alcohol spinning solution and the polyvinyl alcohol spin dope of 35 ﹕ 65 in mass ratio, through wet method or the spinning of dry laminating spining technology, acetalization, makes a kind of Pioloform, polyvinyl acetal conductive fiber that conductive polyvinyl alcohol is cortex of take.
Claims (2)
1. a manufacture method for Pioloform, polyvinyl acetal conductive fiber, is characterized in that this manufacture method adopts following steps:
A) by mass fraction, getting 12-18 part characterization parameter diameter is 0.2-1 μ m, and length is the four acicular type zinc oxide crystal whisker of 5-15 μ m; 3-8 part characterization parameter diameter is 0.2-0.6 μ m, and length is the electric conductivity potassium titanate crystal whisker of 5-12 μ m; After above-mentioned material is mixed, at 300-400 ℃ of vacuum kiln roasting 4-6h; Cooling rear by calgon dispersed with stirring in absolute ethyl alcohol, then atmospheric plasma is processed 10-20min; Then 60-70 ℃ of temperature, containing carrying out ultrasonic wave dispersion in the deionized water of calcium stearate dispersion, cleaning 25-35min, get solution upper strata suspension whisker and remove after filtration the above particle of 16 μ m, and repeat 3-5 time until filtering; After filtering, at vacuum drying oven, dry, obtain modified crystal whiskers mixture;
B) by mass fraction, get steps A) modified crystal whiskers mixture 4-8 part of obtaining, antimony doped tin oxide conducting powder 2-4 part, superconductive carbon black 5-9 part, titanate coupling agent 0.1-0.2 part, aluminate coupling agent 0.1-0.2 part, Tissuemat E 1.5-2.0 part, under 60-70 ℃ of condition, turn/min of mixer 250-400 stirs 45-60min; Obtain modified crystal whiskers conduction blend;
C) by mass fraction, be under the condition that exists at micro-calgon of the modified crystal whiskers conduction blend of 30-45 part, add polyvinyl alcohol spin dope 80-120 part, at 90-95 ℃ of temperature, middling speed stirs 45-60min, obtains conductive polyvinyl alcohol spinning solution;
D) by step C) after conductive polyvinyl alcohol spinning solution mixing under 90-95 ℃ of constant temperature of obtaining, filtration, deaeration, conductive polyvinyl alcohol spinning solution and the polyvinyl alcohol spin dope of 25-35 ﹕ 75-65 in mass ratio, through wet method or the spinning of dry laminating spining technology, acetalization, makes a kind of Pioloform, polyvinyl acetal conductive fiber that conductive polyvinyl alcohol is cortex of take.
2. according to the manufacture method of the Pioloform, polyvinyl acetal conductive fiber described in claim 1, it is characterized in that taking following steps:
A) by mass fraction, getting 15 parts of characterization parameter diameters is 0.2-1 μ m, and length is the four acicular type zinc oxide crystal whisker of 5-15 μ m; 5 parts of characterization parameter diameters are 0.2-0.6 μ m, and length is the electric conductivity potassium titanate crystal whisker of 5-12 μ m; After above-mentioned material is mixed, at 350 ℃ of vacuum kiln roasting 5h; Cooling rear by calgon dispersed with stirring in absolute ethyl alcohol, at atmospheric plasma, process 15min; Then, cleaning 30min loose 65 ℃ of deionized water for ultrasonic wavelength-divisions containing calcium stearate dispersion, gets solution upper strata suspension whisker and removes after filtration the above particle of 16 μ m, and repeat 3-5 time until filtering; After filtering, at vacuum drying oven, dry, obtain modified crystal whiskers mixture;
B) by mass fraction, get steps A) 6 parts, the modified crystal whiskers mixture that obtains, 3 parts of antimony doped tin oxide conducting powder, 7 parts of superconductive carbon blacks, 0.15 part of titanate coupling agent, 0.15 part of aluminate coupling agent, 1.7 parts of Tissuemat Es, under 65 ℃ of conditions, turn/min of mixer 300 stirs 50min; Obtain modified crystal whiskers conduction blend;
C) by mass fraction, be under the condition that exists at micro-calgon of the modified crystal whiskers conduction blend of 40 parts, add 100 parts of polyvinyl alcohol spin dopes, at 92 ℃ of temperature, middling speed stirs 50min, obtains conductive polyvinyl alcohol spinning solution;
D) by step C) after conductive polyvinyl alcohol spinning solution mixing under 92 ℃ of constant temperature of obtaining, filtration, deaeration, conductive polyvinyl alcohol spinning solution and the polyvinyl alcohol spin dope of 30 ﹕ 70 in mass ratio, through wet method or the spinning of dry laminating spining technology, acetalization, makes a kind of Pioloform, polyvinyl acetal conductive fiber that conductive polyvinyl alcohol is cortex of take.
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| CN106380585B (en) * | 2016-08-31 | 2019-01-22 | 浙江理工大学 | A kind of preparation method of antistatic copolyester |
| CN106637467B (en) * | 2016-11-09 | 2018-11-09 | 上海全宇生物科技遂平有限公司 | A kind of boracic nano zine oxide/polyvinyl alcohol composite fiber and preparation method thereof |
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