CN106637467B - A kind of boracic nano zine oxide/polyvinyl alcohol composite fiber and preparation method thereof - Google Patents
A kind of boracic nano zine oxide/polyvinyl alcohol composite fiber and preparation method thereof Download PDFInfo
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- CN106637467B CN106637467B CN201610986204.6A CN201610986204A CN106637467B CN 106637467 B CN106637467 B CN 106637467B CN 201610986204 A CN201610986204 A CN 201610986204A CN 106637467 B CN106637467 B CN 106637467B
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- polyvinyl alcohol
- zine oxide
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/50—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyalcohols, polyacetals or polyketals
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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
Abstract
The present invention provides a kind of boracic nano zine oxide/polyvinyl alcohol composite fibers and preparation method thereof, and the preparation method of the boracic nano zine oxide/polyvinyl alcohol composite fiber includes the following steps：1) polyvinyl alcohol is soluble in water, boric acid is added in heat temperature raising, is uniformly mixed, adds nano zine oxide, after mixing regulation system pH value, and after filtering, deaeration, spinning solution is made；2) spinning solution obtained by step 1) is subjected to the processing of boracic alkaline process wet spinning, neutralized later, wet drawing-off, is heat-treated to obtain Semifinished fibre at washing, then through washing, being drying to obtain.Boracic nano zine oxide/polyvinyl alcohol composite fiber produced by the present invention has excellent mechanical property, anti-microbial property, and preparation method simple process and low cost is honest and clean, is suitable for industrialized production.
Description
Technical field
The present invention relates to a kind of boracic nano zine oxide/polyvinyl alcohol composite fibers and preparation method thereof, belong to polyethylene
Alcohol composite fibre technology field.
Background technology
Nano zine oxide is nontoxic, tasteless, has preferable biocompatibility to skin, and thermal stability is good, this as white,
It can simply be coloured when being fabricated to product, therefore, be often used as the external used medicine of skin, had convergence to skin, disappear
The functions such as inflammation, anti-corrosion, wrinkle resistant and protection.Nano zine oxide can be generated under sunlight very active hydroxyl radical free radical,
Peroxide free radical and O2H free radicals can destroy the proliferative capacity of microbial cell, reach inhibition or kill bacterium
Effect.Nano zine oxide as antiseptic, have many advantages, such as it is nontoxic, long-acting, do not develop immunity to drugs, higher heat resistance, because
And good anti-microbial property is all shown in plastics, coating, fiber.In addition, nano zine oxide acts not only as antiseptic,
It is also used as ultraviolet light screener, is commonly used in cosmetics and fibrous material, so that material obtains anti-ultraviolet performance.
Nano zine oxide as a kind of novel inorganic functional material, daily life and scientific research field have a vast market with it is tempting
Application prospect.
Composite fibre is the physical modification fiber to grow up the 1960s, belongs to one kind of multicomponent fibre, main
It is used for woollen blanket, knitting wool, wool fabric, warming wadding suede filler, silk fabric, non-woven cloth, medical and hygiene article and special work
It takes.The common preparation method of composite fibre has dry method melt spinning and electrostatic spinning at present, and preparation process is more complicated, and
The composite fibre mechanical property of production is poor.Patent publication No is that the Chinese invention patent of CN103388190A discloses a kind of resist
The production method of the degradable polyvinyl of bacterium includes the complexing nano copper dissolution by polyvinyl alcohol, boric acid and 8~12% solid contents 80
In~90 DEG C of hot water, plasticity chelating object is generated as spinning solution, the spinning solution is squeezed out by spinneret, and make ejection
Spinning solidifies in the alkaline coagulating bath that sodium sulphate and sodium hydroxide are formed, and obtains polyvinyl silk, and fiber prepared by the method has
Good degradable and anti-microbial property, but cost is higher, and the mechanical property for generating fiber is poor.Therefore it provides a kind of technique letter
Single, of low cost, the good composite fibre of mechanical property preparation method is extremely urgent.
Invention content
The object of the present invention is to provide a kind of preparation method of boracic nano zine oxide/polyvinyl alcohol composite fiber, the party
Composite fibre made from method can take into account excellent anti-microbial property and mechanical property.
It is compound that second object of the present invention is to provide boracic nano zine oxide/polyvinyl alcohol made from a kind of above method
Fiber.
In order to achieve the goal above, a kind of preparation method of boracic nano zine oxide/polyvinyl alcohol composite fiber of the present invention
Include the following steps：
1) 94~99 parts of polyvinyl alcohol are dissolved in 400~900 parts of water, after being heated to 95~100 DEG C, are added 0.1
~1 part of boric acid, being uniformly mixed makes boric acid be completely dissolved, and obtains poly-vinyl alcohol solution, adds 1~5 part of nano zine oxide, and mixing is equal
Regulation system pH value is 3~6 after even, and after filtering, deaeration, spinning solution is made；
2) spinning solution obtained by step 1) is subjected to wet spinning processing, neutralized later, wet drawing-off, washing, heat treatment
Semifinished fibre is obtained, then through washing, being drying to obtain.
Above-mentioned steps 1) in water used be 40~60 DEG C of warm water.
The nano zine oxide average grain diameter is 30~100nm.
The degree of polymerization of the polyvinyl alcohol is 1700~1800, alcoholysis degree >=99%.
It is hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid, formic acid, acetic acid, acrylic acid, first that the acid used in pH value is adjusted in the step 1)
Any one in base acrylic acid, polyacrylic acid, polymethylacrylic acid, ascorbic acid or arbitrary combination；Alkali used is hydrogen-oxygen
Change sodium, potassium hydroxide, diethanol amine, triethanolamine, ethyl alcohol sodium sulfonate, in disodium ethylene diamine tetraacetate any one or it is arbitrary
Combination.
It is to stir and evenly mix that the mode being uniformly mixed after nano zine oxide, which is added, in the step 1), and mixing time is 2~4h.
The sum of polyvinyl alcohol and nano zine oxide mass concentration are 10~20% in gained spinning solution in the step 1).
In the step 2) wet spinning handle when use saltcake coagulating bath, wherein the mass concentration of sodium sulphate be 340~
420g/L。
The temperature of the saltcake coagulating bath is 40~50 DEG C, and pH value is 8~12.
Wet drawing-off is 1.5~2 times of drawing-off in 88~92 DEG C of saltcake coagulating baths in the step 2), wherein sodium sulphate
Mass concentration is 350~390g/L.
Heat treatment is to stretch 1.5~2 times under the conditions of xeothermic 210~220 DEG C in the step 2).
Gained boracic nano zine oxide/polyvinyl alcohol composite fiber carries out oiling treatment or cut-off part in the step 2)
Reason carries out cutoff process after oiling treatment.
The technical solution of boracic nano zine oxide/polyvinyl alcohol composite fiber of the present invention is as follows：
A kind of boracic nano zine oxide/polyvinyl alcohol composite fiber is made using the above method.
Raw materials used boracic nano zine oxide/polyvinyl alcohol composite fiber preparation process of the present invention is convenient source, is come
Source is extensive, cheap, and technological process is simple, and equipment investment is small, and cost low yield is big, it is easy to accomplish industrialized production.
Boracic nano zine oxide/polyvinyl alcohol composite fiber preparation process of the present invention has used nano zine oxide, nano oxygen
It is nontoxic, tasteless to change zinc, has preferable biocompatibility to skin, has the function of inhibiting or killing bacterium.In addition, using this hair
The boracic nano zine oxide that the bright boracic nano zine oxide/polyvinyl alcohol composite fiber preparation method obtains/compound fibre of polyvinyl alcohol
Tie up the mechanical property having had：For fiber number in 1.42~1.55dtex, it is 6.50~8.50cN/dtex, introductory die to do fracture strength
Amount reaches 130~150cN/dtex.
Specific implementation mode
With reference to specific embodiment, invention is further described in detail.
Embodiment 1
The present embodiment boracic nano zine oxide/polyvinyl alcohol composite fiber is mainly made of the component of following mass fraction：
1 part of nano zine oxide, 99 parts of polyvinyl alcohol, 0.6 part of boric acid, wherein nano zine oxide average grain diameter are 35nm, polyvinyl alcohol
The degree of polymerization is 1700~1800, alcoholysis degree >=99%.
The preparation method of the boracic nano zine oxide/polyvinyl alcohol composite fiber includes the following steps：
1) 99 parts of polyvinyl alcohol are dissolved in the water that 900 parts of temperature are 50 DEG C, after being heated to 95 DEG C, keep system temperature
Spend it is constant, later while stirring be added 0.6 part of boric acid, stir to poly-vinyl alcohol solution is completely dissolved to obtain, add 1 part of nano oxygen
Change zinc, be sufficiently stirred 2h, after mixing, it is 4 that hydrochloric acid regulation system pH value, which is added, after filtering, standing and defoaming 6h, is made poly-
The spinning solution that the sum of vinyl alcohol and nano zine oxide mass concentration are 10%；
2) spinning solution obtained by step 1) is subjected to wet spinning processing, the saltcake coagulating bath in order to control of specific experiment parameter
(a concentration of 380g/L of sodium sulfate quality) temperature is 44 DEG C, pH value 10；Neutralized later, wet drawing-off, washing are heat-treated partly
Finished fiber, wherein wet drawing-off is 1.5 times of the drawing-off in 90 DEG C of metabisulfite solution (mass concentration 370g/L), heat treatment
It is to stretch 1.5 times at xeothermic 210 DEG C；Gained Semifinished fibre again through washing, drying, oil, cut off to get.
Embodiment 2
The present embodiment boracic nano zine oxide/polyvinyl alcohol composite fiber is mainly made of the component of following mass fraction：
1.5 parts of nano zine oxide, 99 parts of polyvinyl alcohol, 0.6 part of boric acid, wherein nano zine oxide average grain diameter are 35nm, polyvinyl alcohol
The degree of polymerization be 1700~1800, alcoholysis degree >=99%.
The preparation method of the boracic nano zine oxide/polyvinyl alcohol composite fiber includes the following steps：
1) 99 parts of polyvinyl alcohol are dissolved in the water that 900 parts of temperature are 50 DEG C, after being heated to 95 DEG C, keep system temperature
Spend it is constant, later while stirring be added 0.6 part of boric acid, stir to poly-vinyl alcohol solution is completely dissolved to obtain, add 1.5 parts of nanometers
Zinc oxide is sufficiently stirred 3h, and after mixing, it is 4 that formic acid regulation system pH value, which is added, after filtering, standing and defoaming 6h, is made
The spinning solution that the sum of polyvinyl alcohol and nano zine oxide mass concentration are 10%；
2) spinning solution obtained by step 1) is subjected to wet spinning processing, the saltcake coagulating bath in order to control of specific experiment parameter
(a concentration of 340g/L of sodium sulfate quality) temperature is 44 DEG C, pH value 10；Neutralized later, wet drawing-off, washing are heat-treated partly
Finished fiber, wherein wet drawing-off is 1.5 times of the drawing-off in 90 DEG C of metabisulfite solution (mass concentration 350g/L), heat treatment
It is to stretch 1.5 times at xeothermic 210 DEG C；Gained Semifinished fibre again through washing, drying, oil, cut off to get.
Embodiment 3
The present embodiment boracic nano zine oxide/polyvinyl alcohol composite fiber is mainly made of the component of following mass fraction：
1 part of nano zine oxide, 99 parts of polyvinyl alcohol, 0.6 part of boric acid, wherein nano zine oxide average grain diameter are 48nm, polyvinyl alcohol
The degree of polymerization is 1700~1800, alcoholysis degree >=99%.
The preparation method of the boracic nano zine oxide/polyvinyl alcohol composite fiber includes the following steps：
1) 99 parts of polyvinyl alcohol are dissolved in the water that 900 parts of temperature are 50 DEG C, after being heated to 95 DEG C, keep system temperature
Spend it is constant, later while stirring be added 0.6 part of boric acid, stir to poly-vinyl alcohol solution is completely dissolved to obtain, add 1 part of nano oxygen
Change zinc, is sufficiently stirred 4h, after mixing, it is 4 that ascorbic acid regulation system pH value, which is added, after filtering, standing and defoaming 6h, system
Obtain the spinning solution that the sum of polyvinyl alcohol and nano zine oxide mass concentration are 10%；
2) spinning solution obtained by step 1) is subjected to wet spinning processing, the saltcake coagulating bath in order to control of specific experiment parameter
(a concentration of 420g/L of sodium sulfate quality) temperature is 44 DEG C, pH value 10；Neutralized later, wet drawing-off, washing are heat-treated partly
Finished fiber, wherein wet drawing-off is 1.5 times of the drawing-off in 90 DEG C of metabisulfite solution (mass concentration 390g/L), heat treatment
It is to stretch 1.5 times at xeothermic 210 DEG C；Gained Semifinished fibre again through washing, drying, oil, cut off to get.
Embodiment 4
The present embodiment boracic nano zine oxide/polyvinyl alcohol composite fiber is mainly made of the component of following mass fraction：
1.5 parts of nano zine oxide, 99 parts of polyvinyl alcohol, 0.6 part of boric acid, wherein nano zine oxide average grain diameter are 48nm, polyvinyl alcohol
The degree of polymerization be 1700~1800, alcoholysis degree >=99%.
The preparation method of the boracic nano zine oxide/polyvinyl alcohol composite fiber includes the following steps：
1) 99 parts of polyvinyl alcohol are dissolved in the water that 900 parts of temperature are 50 DEG C, after being heated to 95 DEG C, keep system temperature
Spend it is constant, later while stirring be added 0.6 part of boric acid, stir to poly-vinyl alcohol solution is completely dissolved to obtain, add 1.5 parts of nanometers
Zinc oxide is sufficiently stirred 2.5h, and after mixing, it is 4 that polyacrylic acid regulation system pH value, which is added, through filtering, standing and defoaming 6h
Afterwards, the spinning solution that the sum of polyvinyl alcohol and nano zine oxide mass concentration are 10% is made；
2) spinning solution obtained by step 1) is subjected to wet spinning processing, the saltcake coagulating bath in order to control of specific experiment parameter
(a concentration of 390g/L of sodium sulfate quality) temperature is 44 DEG C, pH value 10；Neutralized later, wet drawing-off, washing are heat-treated partly
Finished fiber, wherein wet drawing-off is 1.5 times of the drawing-off in 90 DEG C of metabisulfite solution (mass concentration 360g/L), heat treatment
It is to stretch 1.5 times at xeothermic 210 DEG C；Gained Semifinished fibre again through washing, drying, oil, cut off to get.
Embodiment 5
The present embodiment boracic nano zine oxide/polyvinyl alcohol composite fiber is mainly made of the component of following mass fraction：
1 part of nano zine oxide, 99 parts of polyvinyl alcohol, 0.1 part of boric acid, wherein nano zine oxide average grain diameter are 60nm, polyvinyl alcohol
The degree of polymerization is 1700~1800, alcoholysis degree >=99%.
The preparation method of the boracic nano zine oxide/polyvinyl alcohol composite fiber includes the following steps：
1) 99 parts of polyvinyl alcohol are dissolved in the water that 400 parts of temperature are 40 DEG C, after being heated to 96 DEG C, keep system temperature
Spend it is constant, later while stirring be added 0.1 part of boric acid, stir to poly-vinyl alcohol solution is completely dissolved to obtain, add 1 part of nano oxygen
Change zinc, be sufficiently stirred 3h, after mixing, it is 3 that sulfuric acid regulation system pH value, which is added, after filtering, standing and defoaming 6h, is made poly-
The spinning solution that the sum of vinyl alcohol and nano zine oxide mass concentration are 20%；
2) spinning solution obtained by step 1) is subjected to wet spinning processing, the saltcake coagulating bath in order to control of specific experiment parameter
(a concentration of 350g/L of sodium sulfate quality) temperature is 40 DEG C, pH value 8；Neutralized later, wet drawing-off, washing are heat-treated partly
Finished fiber, wherein wet drawing-off is that 2 times of drawing-off, heat treatment are in 88 DEG C of metabisulfite solution (mass concentration 380g/L)
At xeothermic 213 DEG C, 1.8 times are stretched；Gained Semifinished fibre again through washing, drying, oil, cut off to get.
Embodiment 6
The present embodiment boracic nano zine oxide/polyvinyl alcohol composite fiber is mainly made of the component of following mass fraction：
1.5 parts of nano zine oxide, 98.5 parts of polyvinyl alcohol, 0.3 part of boric acid, wherein nano zine oxide average grain diameter are 60nm, polyethylene
The degree of polymerization of alcohol is 1700~1800, alcoholysis degree >=99%.
The preparation method of the boracic nano zine oxide/polyvinyl alcohol composite fiber includes the following steps：
1) 98.5 parts of polyvinyl alcohol are dissolved in the water that 426 parts of temperature are 47 DEG C, after being heated to 97 DEG C, keep system
Temperature is constant, and 0.3 part of boric acid is added while stirring later, stirs to poly-vinyl alcohol solution is completely dissolved to obtain, adds 1.5 parts and receive
Rice zinc oxide, is sufficiently stirred 4h, and after mixing, it is 3.5 that methacrylic acid regulation system pH value, which is added, de- through filtering, standing
After steeping 6h, the spinning solution that the sum of polyvinyl alcohol and nano zine oxide mass concentration are 19% is made；
2) spinning solution obtained by step 1) is subjected to wet spinning processing, the saltcake coagulating bath in order to control of specific experiment parameter
(a concentration of 360g/L of sodium sulfate quality) temperature is 41 DEG C, pH value 11；Neutralized later, wet drawing-off, washing are heat-treated partly
Finished fiber, wherein wet drawing-off is 1.7 times of the drawing-off in 92 DEG C of metabisulfite solution (mass concentration 355g/L), heat treatment
It is to stretch 1.9 times at xeothermic 220 DEG C；Gained Semifinished fibre again through washing, drying, oil, cut off to get.
Embodiment 7
The present embodiment boracic nano zine oxide/polyvinyl alcohol composite fiber is mainly made of the component of following mass fraction：
2 parts of nano zine oxide, 98 parts of polyvinyl alcohol, 0.4 part of boric acid, wherein nano zine oxide average grain diameter are 60nm, polyvinyl alcohol
The degree of polymerization is 1700~1800, alcoholysis degree >=99%.
The preparation method of the boracic nano zine oxide/polyvinyl alcohol composite fiber includes the following steps：
1) 98 parts of polyvinyl alcohol are dissolved in the water that 482 parts of temperature are 49 DEG C, after being heated to 98 DEG C, keep system temperature
Spend it is constant, later while stirring be added 0.4 part of boric acid, stir to poly-vinyl alcohol solution is completely dissolved to obtain, add 2 parts of nano oxygens
Change zinc, is sufficiently stirred 3h, after mixing, it is 4.5 that acrylic acid regulation system pH value, which is added, after filtering, standing and defoaming 6h, system
Obtain the spinning solution that the sum of polyvinyl alcohol and nano zine oxide mass concentration are 17%；
2) spinning solution obtained by step 1) is subjected to wet spinning processing, the saltcake coagulating bath in order to control of specific experiment parameter
(a concentration of 370g/L of sodium sulfate quality) temperature is 42 DEG C, pH value 9；Neutralized later, wet drawing-off, washing are heat-treated partly
Finished fiber, wherein wet drawing-off is 1.8 times of the drawing-off in 89 DEG C of metabisulfite solution (mass concentration 365g/L), heat treatment
It is to stretch 2 times at xeothermic 215 DEG C；Gained Semifinished fibre again through washing, drying, oil, cut off to get.
Embodiment 8
The present embodiment boracic nano zine oxide/polyvinyl alcohol composite fiber is mainly made of the component of following mass fraction：
1 part of nano zine oxide, 98.5 parts of polyvinyl alcohol, 0.7 part of boric acid, wherein nano zine oxide average grain diameter are 100nm, polyvinyl alcohol
The degree of polymerization be 1700~1800, alcoholysis degree >=99%.
The preparation method of the boracic nano zine oxide/polyvinyl alcohol composite fiber includes the following steps：
1) 98.5 parts of polyvinyl alcohol are dissolved in the water that 567 parts of temperature are 55 DEG C, after being heated to 99 DEG C, keep system
Temperature is constant, and 0.7 part of boric acid is added while stirring later, stirs to poly-vinyl alcohol solution is completely dissolved to obtain, adds 1 part of nanometer
Zinc oxide is sufficiently stirred 3.5h, and after mixing, it is 5 that diethanol amine regulation system pH value, which is added, through filtering, standing and defoaming 6h
Afterwards, the spinning solution that the sum of polyvinyl alcohol and nano zine oxide mass concentration are 15% is made；
2) spinning solution obtained by step 1) is subjected to wet spinning processing, the saltcake coagulating bath in order to control of specific experiment parameter
(a concentration of 400g/L of sodium sulfate quality) temperature is 43 DEG C, pH value 10；Neutralized later, wet drawing-off, washing are heat-treated partly
Finished fiber, wherein wet drawing-off is 1.6 times of the drawing-off in 91 DEG C of metabisulfite solution (mass concentration 375g/L), heat treatment
It is to stretch 2 times at xeothermic 217 DEG C；Gained Semifinished fibre again through washing, drying, oil, cut off to get.
Embodiment 9
The present embodiment boracic nano zine oxide/polyvinyl alcohol composite fiber is mainly made of the component of following mass fraction：
1.5 parts of nano zine oxide, 98.5 parts of polyvinyl alcohol, 0.8 part of boric acid, wherein nano zine oxide average grain diameter are 100nm, polyethylene
The degree of polymerization of alcohol is 1700~1800, alcoholysis degree >=99%.
The preparation method of the boracic nano zine oxide/polyvinyl alcohol composite fiber includes the following steps：
1) 98.5 parts of polyvinyl alcohol are dissolved in the water that 669 parts of temperature are 58 DEG C, after being heated to 100 DEG C, keeping body
It is that temperature is constant, 0.8 part of boric acid is added while stirring later, stirs to poly-vinyl alcohol solution is completely dissolved to obtain, add 1.5 parts
Nano zine oxide is sufficiently stirred 2h, and after mixing, it is 4.8 that disodium ethylene diamine tetraacetate regulation system pH value, which is added, is passed through
After filter, standing and defoaming 6h, the spinning solution that the sum of polyvinyl alcohol and nano zine oxide mass concentration are 13% is made；
2) spinning solution obtained by step 1) is subjected to wet spinning processing, the saltcake coagulating bath in order to control of specific experiment parameter
(a concentration of 410g/L of sodium sulfate quality) temperature is 45 DEG C, pH value 12；Neutralized later, wet drawing-off, washing are heat-treated partly
Finished fiber, wherein wet drawing-off is 1.9 times of the drawing-off in 89 DEG C of metabisulfite solution (mass concentration 385g/L), heat treatment
It is to stretch 2 times at xeothermic 219 DEG C；Gained Semifinished fibre again through washing, drying, oil, cut off to get.
Embodiment 10
The present embodiment boracic nano zine oxide/polyvinyl alcohol composite fiber is mainly made of the component of following mass fraction：
3 parts of nano zine oxide, 94 parts of polyvinyl alcohol, 0.9 part of boric acid, wherein nano zine oxide average grain diameter are 30nm, polyvinyl alcohol
The degree of polymerization is 1700~1800, alcoholysis degree >=99%.
The preparation method of the boracic nano zine oxide/polyvinyl alcohol composite fiber includes the following steps：
1) 94 parts of polyvinyl alcohol are dissolved in the water that 733 parts of temperature are 60 DEG C, after being heated to 99 DEG C, keep system temperature
Spend it is constant, later while stirring be added 0.9 part of boric acid, stir to poly-vinyl alcohol solution is completely dissolved to obtain, add 3 parts of nano oxygens
Change zinc, is sufficiently stirred 4h, after mixing, it is 4.3 that sodium hydroxide regulation system pH value, which is added, after filtering, standing and defoaming 6h,
The spinning solution that the sum of polyvinyl alcohol and nano zine oxide mass concentration are 12% is made；
2) spinning solution obtained by step 1) is subjected to wet spinning processing, the saltcake coagulating bath in order to control of specific experiment parameter
(a concentration of 420g/L of sodium sulfate quality) temperature is 47 DEG C, pH value 11；Neutralized later, wet drawing-off, washing are heat-treated partly
Finished fiber, wherein wet drawing-off is that 2 times of drawing-off, heat treatment are in 92 DEG C of metabisulfite solution (mass concentration 390g/L)
At xeothermic 214 DEG C, 1.6 times are stretched；Gained Semifinished fibre again through washing, drying, oil, cut off to get.
Embodiment 11
The present embodiment boracic nano zine oxide/polyvinyl alcohol composite fiber is mainly made of the component of following mass fraction：
5 parts of nano zine oxide, 96 parts of polyvinyl alcohol, 1.0 parts of boric acid, wherein nano zine oxide average grain diameter are 30nm, polyvinyl alcohol
The degree of polymerization is 1700~1800, alcoholysis degree >=99%.
The preparation method of the boracic nano zine oxide/polyvinyl alcohol composite fiber includes the following steps：
1) 96 parts of polyvinyl alcohol are dissolved in the water that 809 parts of temperature are 53 DEG C, after being heated to 100 DEG C, keep system
Temperature is constant, and 1.0 parts of boric acid are added while stirring later, stirs to poly-vinyl alcohol solution is completely dissolved to obtain, adds 5 parts of nanometers
Zinc oxide is sufficiently stirred 4h, and after mixing, it is 3.7 that ethyl alcohol sodium sulfonate regulation system pH value, which is added, through filtering, standing and defoaming
After 6h, the spinning solution that the sum of polyvinyl alcohol and nano zine oxide mass concentration are 11% is made；
2) spinning solution obtained by step 1) is subjected to wet spinning processing, the saltcake coagulating bath in order to control of specific experiment parameter
(a concentration of 340g/L of sodium sulfate quality) temperature is 50 DEG C, pH value 8；Neutralized later, wet drawing-off, washing are heat-treated partly
Finished fiber, wherein wet drawing-off is 1.5 times of the drawing-off in 88 DEG C of metabisulfite solution (mass concentration 350g/L), heat treatment
It is to stretch 1.7 times at xeothermic 220 DEG C；Gained Semifinished fibre again through washing, drying, oil, cut off to get.
Comparative example
This comparative example polyvinyl alcohol composite fiber is mainly made of 100kg polyvinyl alcohol.
The preparation method of the polyvinyl alcohol composite fiber includes the following steps：
1) 100kg polyvinyl alcohol is dissolved in the water that 700kg temperature is 50 DEG C, after being heated to 90 DEG C, is stirred to complete
Fully dissolved obtains poly-vinyl alcohol solution, and it is 7.5 that sodium hydroxide regulation system pH value, which is added, continues to heat maintenance system temperature to be 95
DEG C, after filtering, standing and defoaming 6h, the spinning solution that polyvinyl alcohol mass concentration is 18% is made；
2) spinning solution obtained by step 1) is subjected to wet spinning processing, the saltcake coagulating bath in order to control of specific experiment parameter
(a concentration of 380g/L of sodium sulfate quality) temperature is 50 DEG C, pH value 6.5；Neutralized later, wet drawing-off, is heat-treated washing
Semifinished fibre, wherein wet drawing-off is 1.5 times of the drawing-off in 90 DEG C of metabisulfite solution (mass concentration 370g/L), at heat
Reason is to stretch 1.5 times at xeothermic 210 DEG C；Gained Semifinished fibre again through washing, drying, oil, cut off to get.
Experimental example
This experimental example has detected the mechanical property of the composite fibre obtained by embodiment 1~11 and comparative example, gained experiment
The results are shown in Table 1.
The mechanical performance data table of composite fibre obtained by 1 embodiment 1~11 of table and comparative example
From table 1 it follows that the mechanical strength of the composite fibre obtained by the embodiment of the present invention 1~11 is substantially better than pair
Ratio illustrates the excellent in mechanical performance of boracic nano zine oxide/polyvinyl alcohol composite fiber obtained by technical solution of the present invention, energy
Enough meet industrial processes requirement.
Claims (6)
1. a kind of preparation method of boracic nano zine oxide/polyvinyl alcohol composite fiber, which is characterized in that include the following steps：
1）94 ~ 99 parts of polyvinyl alcohol are dissolved in 400 ~ 900 parts of water, after being heated to 95 ~ 100 DEG C, 0.1 ~ 1 part of boron is added
Acid, being uniformly mixed makes boric acid be completely dissolved, and obtains poly-vinyl alcohol solution, adds 1 ~ 5 part of nano zine oxide, adjust after mixing
System pH is 3 ~ 6, and after filtering, deaeration, spinning solution is made；
2）By step 1）Gained spinning solution carries out wet spinning processing, and neutralized later, wet drawing-off, washing are heat-treated partly
Finished fiber, then through washing, being drying to obtain；
Step 2）Saltcake coagulating bath is used when middle wet spinning processing, the wherein mass concentration of sodium sulphate is 340 ~ 420g/L；Institute
The temperature for stating saltcake coagulating bath is 40 ~ 50 DEG C, and pH value is 8 ~ 12；
Step 2）In wet drawing-off be 1.5 ~ 2 times of drawing-off in 88 ~ 92 DEG C of saltcake coagulating baths, wherein the mass concentration of sodium sulphate is
350~390g/L；
Step 2）Middle heat treatment is to stretch 1.5 ~ 2 times under the conditions of xeothermic 210 ~ 220 DEG C.
2. the preparation method of boracic nano zine oxide/polyvinyl alcohol composite fiber according to claim 1, feature exist
In the nano zine oxide average grain diameter is 30 ~ 100nm.
3. the preparation method of boracic nano zine oxide/polyvinyl alcohol composite fiber according to claim 1, feature exist
In the degree of polymerization of the polyvinyl alcohol is 1700 ~ 1800, alcoholysis degree >=99%.
4. the preparation method of boracic nano zine oxide/polyvinyl alcohol composite fiber according to claim 1, feature exist
In step 1）Acid used in middle adjusting pH value be hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid, formic acid, acetic acid, acrylic acid, methacrylic acid,
Any one in polyacrylic acid, polymethylacrylic acid, ascorbic acid or arbitrary combination；Alkali used is sodium hydroxide, hydrogen-oxygen
Change any one in potassium, diethanol amine, triethanolamine, ethyl alcohol sodium sulfonate, disodium ethylene diamine tetraacetate or arbitrary combination.
5. the preparation method of boracic nano zine oxide/polyvinyl alcohol composite fiber according to claim 1, feature exist
In step 1）It is to stir and evenly mix that the mode being uniformly mixed after nano zine oxide, which is added, and mixing time is 2 ~ 4h.
6. a kind of boracic nano zine oxide/polyvinyl alcohol composite fiber, which is characterized in that using such as any one of claim 1 ~ 5
The preparation method of the boracic nano zine oxide/polyvinyl alcohol composite fiber is made.
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