CN103046153B - Preparation method of polyvinyl acetal negative oxygen ion fibers - Google Patents
Preparation method of polyvinyl acetal negative oxygen ion fibers Download PDFInfo
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- 239000000835 fiber Substances 0.000 title claims abstract description 42
- 239000001301 oxygen Substances 0.000 title claims abstract description 36
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 36
- 229920002554 vinyl polymer Polymers 0.000 title claims abstract description 20
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 125000002777 acetyl group Chemical class [H]C([H])([H])C(*)=O 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title abstract 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 35
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 35
- 238000001914 filtration Methods 0.000 claims abstract description 33
- -1 oxygen ion Chemical class 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 30
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims abstract description 23
- 238000009987 spinning Methods 0.000 claims abstract description 21
- 229940070527 tourmaline Drugs 0.000 claims abstract description 16
- 229910052613 tourmaline Inorganic materials 0.000 claims abstract description 16
- 239000011032 tourmaline Substances 0.000 claims abstract description 16
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000011591 potassium Substances 0.000 claims abstract description 13
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 13
- 229910052625 palygorskite Inorganic materials 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000006359 acetalization reaction Methods 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims description 36
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 33
- 238000003756 stirring Methods 0.000 claims description 32
- 239000013078 crystal Substances 0.000 claims description 28
- 238000012512 characterization method Methods 0.000 claims description 24
- 238000004519 manufacturing process Methods 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 16
- 239000007822 coupling agent Substances 0.000 claims description 16
- 229920002978 Vinylon Polymers 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 11
- 230000002269 spontaneous effect Effects 0.000 claims description 10
- 239000004067 bulking agent Substances 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
- 238000006243 chemical reaction Methods 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
- 238000000578 dry spinning Methods 0.000 claims description 8
- 235000019441 ethanol Nutrition 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
- 238000004381 surface treatment Methods 0.000 claims description 8
- 239000004094 surface-active agent Substances 0.000 claims description 8
- 239000000725 suspension Substances 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
- 239000002131 composite material Substances 0.000 abstract 1
- 238000007872 degassing Methods 0.000 abstract 1
- 229920000742 Cotton Polymers 0.000 description 6
- 239000000126 substance Substances 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 3
- 238000003915 air pollution Methods 0.000 description 2
- 230000002079 cooperative effect Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
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- 238000009941 weaving Methods 0.000 description 2
- 229920000297 Rayon Polymers 0.000 description 1
- 238000004378 air conditioning Methods 0.000 description 1
- 229910052925 anhydrite Inorganic materials 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
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- 238000004332 deodorization Methods 0.000 description 1
- 230000001877 deodorizing effect Effects 0.000 description 1
- 238000001784 detoxification Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
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- 230000036541 health Effects 0.000 description 1
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- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 230000004630 mental health Effects 0.000 description 1
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- 230000035699 permeability Effects 0.000 description 1
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- 229920001281 polyalkylene Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
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- 238000001179 sorption measurement Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
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- 229920002994 synthetic fiber Polymers 0.000 description 1
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Abstract
The invention discloses a preparation method of polyvinyl acetal negative oxygen ion fibers. The preparation method comprises the following steps of: adding calcium sulfate whiskers, nanometre palygorskite fibers, potassium tetratitanate whiskers and tourmaline composite powder in a fiber grade polyvinyl alcohol spinning solution to be prepared into a tourmaline polyvinyl alcohol spinning solution, then mixing, filtering, carrying out degassing, spinning by a wet method or a dry method and an acetalization treatment to be prepared into negative oxygen ion polyvinyl acetal fibers. The fibres comprise filaments and short fibers; the negative oxygen ion polyvinyl acetal fibers have good strength, stiffness degree and wear resistance, and further can stimulate the release of more negative oxygen ions.
Description
Technical field
The present invention relates to a kind of manufacture method of polyvinyl alcohol (PVA) acetal negative oxygen ion fiber of Spontaneous release negative oxygen ion function, the manufacture method that comprises fibre-grade polyvinyl alcohol (PVA), calcium sulfate (CaSO4) whisker, nanometer palygorskite fiber, potassium tetratitanate (K20.4Ti02) whisker, composition tourmaline powder body fiber, belongs to chemical fibre manufacturing technology.
Background technology
The fiber making as raw material spinning taking polyvinyl alcohol, by this fiber, through vinylon that formaldehyde treated obtains, 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 staple fibre in a large number in order to cotton blending, with viscose or with other fiber blends or pure spinning, manufacture knitted fabric, the woven fabrics such as coat and shirt, cotton sweater and trousers, sweater, household textiles, bedding.
Polyvinyl has good hygroscopicity, gas permeability, flexibility, comfortable and easy to wear; There is the smooth characteristic such as nice and cool, antistatic, be widely used at present the fields such as clothes, family spin, non-weaving cloth.Along with scientific and technical development, the various new type functional vinylons taking polyvinyl alcohol as raw material are continually developed successfully, have further expanded application market.Functional polyalkylene vinyl acetal fiber can be divided into according to its function: as fire-retardant, antibacterial, negative oxygen ion, far infrared, conductive polyvinyl alcohol acetal fibre etc.
Whisker be with monocrystalline form grow the diameter very little (0.1～10um), atomic arrangement high-sequential, the intensity that form approach perfect crystal theoretical value, have the fibrous material of certain draw ratio (5～1000).Potassium Tetratitanate Whisker is a kind of staple fibre compound of novel needle-like, and because its size is tiny, perfect crystalline, has splendid mechanical property, physical property, stable chemical property, the excellent feature such as corrosion resistance, ABRASION RESISTANCE.Calcium sulfate crystal whiskers is to have fibrous (must shape) monocrystal, integrates the two advantage of fortifying fibre and ultra-fine inorganic filler, can be used for doing in macromolecular material strengthening and toughening agent or functional stuffing; Be a kind of Application Areas more extensively, extremely rising inorganic salts whisker.
Palygorskite is needle-like, fibrous, bar-shaped under electron microscope.Crystals is multi-pore channel, there is very large specific area and adsorption capacity, have good rheological characteristic and catalytic performance, the very strong sterilizing of tool, deodorizing, detoxification, killing ability, be a kind of desirable macromolecular material reinforcing agent and macromolecular material functional modifier, have a wide range of applications field.
Tourmaline has unique physical and chemical performance such as piezoelectricity and pyroelectricity, when the variation of temperature, humidity and pressure etc. can cause the electrical potential difference of tourmaline crystal, making surrounding air that ionization occur is in air, to produce negative oxygen ion, thereby reach the object purifying air, be widely used in recent years the fields such as functional fibre, weaving, clothes, family life articles for use.In chemical fibre, add tourmaline powder, can make fiber there is far-infrared ray warming function, deodorization functions, anion emission function and antibacterial functions, be referred to as " singular fibre ".
Air negative oxgyen ion has health-care function to human body, environment is played purify air, the effect of antibacterial and deodouring.Along with the modernization of indoor decoration decoration, room air pollution has become the common problem of paying close attention in whole world various countries, and environmentalist has been listed room air pollution in one of factor to people's health hazard maximum.Expert's research shows. serious 2～5 times than outdoor air of the pollution levels of room air, can reach 100 times under special circumstances; 25/cm of air-anion concentration ﹤ in the sealing chamber of dress air-conditioning
3.World Health Organization's regulation, the negative oxygen ion content in fresh air should be lower than 1000～5000/cm
3; Concerning the mankind, airborne negative oxygen ion is important just as the vitamin in food; Negative oxygen ion is that non-ordinary light is bright as its DEVELOPMENT PROSPECT of a kind of resource, in polyvinyl alcohol, add potassium tetratitanate (K20.4Ti02) whisker of composition tourmaline powder body and cooperative effect etc., exploitation the taking of negative oxygen ion function, Indoor Textiles, to improving people's air quality of subenvironment around, promote healthy very valuable and meaning.
Summary of the invention
The object of the invention is to overcome the deficiency that prior art exists, a kind of manufacture method of the Pioloform, polyvinyl acetal negative oxygen ion fiber with Spontaneous release negative oxygen ion function is provided.
The object of the invention is to complete by following technical solution, real name is invented the manufacture method of described Pioloform, polyvinyl acetal negative oxygen ion fiber, and this manufacture method adopts following steps:
A) getting 8-12 part characterization parameter diameter by mass fraction is 0.1-0.8um, the palygorskite fiber that length is 6-15um; 3-5 part characterization parameter diameter is 0.3-1um, the calcium sulfate crystal whiskers that length is 6-15um, and 4-6 part characterization parameter diameter is 0.5-1um, the Potassium Tetratitanate Whisker that length is 5-15um; After above-mentioned three materials are mixed, at 250-350 DEG C of vacuum kiln roasting 4-6h; Cooling rear by calgon dispersed with stirring in absolute ethyl alcohol, under atmospheric pressure state, carry out Surface Treatment with Plasma 10-20min; Then, cleaning 25-35min loose 60-70 DEG C of deionized water for ultrasonic wavelength-division, gets solution upper strata suspension whisker and removes after filtration the above particle of 16um, and repeat 3-5 time until filtering; After filtering, dry at vacuum drying oven, obtain modified crystal whiskers mixture;
B) get 0.8-1.2 part titanate coupling agent by mass fraction and dilute, be heated to 40-50 DEG C at 1.5-2.5 part alcohol solution; By titanate coupling agent weak solution and steps A) 8-12 part modified crystal whiskers mixture of obtaining stirs 30-45min in mixer under 70-80 DEG C of condition; Dry; Then add nanoscale composition tourmaline powder 8-12 part, EPP bulking agent 1-2 part, surfactant calcium stearate 0.3-0.7 part, airtight stirring reaction 30-45min in mixer under 60-70 DEG C of condition; Add polyvinyl alcohol spin dope 80-120 part, turn/min of 150-200 speed stirs 45-60min, obtains modified polyvinylalcohol spinning solution blend again;
C) by step B) mixing under 90-95 DEG C of constant temperature of modified polyvinylalcohol spinning solution, filtration, the deaeration that obtain, by wet method or dry spinning, acetalization, makes a kind of Spontaneous release negative oxygen ion vinylon.
The manufacture method of Pioloform, polyvinyl acetal negative oxygen ion fiber of the present invention, it adopts following optimal technical scheme to be:
A) getting 10 parts of characterization parameter diameters by mass fraction is 0.1-0.8um, the palygorskite fiber that length is 6-15um; 4 parts of characterization parameter diameters are 0.3-1um, the calcium sulfate crystal whiskers that length is 6-15um, and 5 parts of characterization parameter diameters are 0.5-1um, the Potassium Tetratitanate Whisker that length is 5-15um; After above-mentioned three materials are mixed, at 300 DEG C of vacuum kiln roasting 5h; Cooling rear by calgon dispersed with stirring in absolute ethyl alcohol, under atmospheric pressure state, carry out Surface Treatment with Plasma 15min; Then, cleaning 30min loose 65 DEG C of deionized water for ultrasonic wavelength-divisions, gets solution upper strata suspension whisker and removes after filtration the above particle of 16um, and repeat 4 times until filtering; After filtering, dry at vacuum drying oven, obtain modified crystal whiskers mixture;
B) getting 1.0 parts of titanate coupling agents by mass fraction dilutes at 2 parts of alcohol solutions, is heated to 45 DEG C; By titanate coupling agent weak solution and steps A) 10 parts of modified crystal whiskers mixtures obtaining stir 40min in mixer under 75 DEG C of conditions; Dry; Then add 10 parts of nanoscale composition tourmaline powders, 1.5 parts of EPP bulking agents, 0.5 part of surfactant calcium stearate, airtight stirring reaction 40min in mixer under 65 DEG C of conditions; Add 100 parts of polyvinyl alcohol spin dopes, 180 turn/min speed stir 50min, obtain modified polyvinylalcohol spinning solution blend again;
C) by step B) mixing under 92 DEG C of constant temperature of modified polyvinylalcohol spinning solution, filtration, the deaeration that obtain, by wet method or dry spinning, acetalization, makes a kind of Spontaneous release negative oxygen ion vinylon.
The present invention is Potassium Tetratitanate Whisker, the nanometer palygorskite fiber that adds nano level composition tourmaline powder and cooperative effect thereof in polyvinyl alcohol, and this inorganic material can be improved the intensity of vinylon, well-pressed degree, ABRASION RESISTANCE; Can also excite the more negative oxygen ions of release; This negative oxygen ion vinylon can be widely used in that clothes, bedding, family are spun and drapery etc., and produces the negative oxygen ion of higher concentration; Make people carefree and leisurely comfortable, relaxed and joyful as lived in oxygen bar or beach, forest, and promote physical and mental health, increase work efficiency.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be described in detail: the manufacture method of a kind of Pioloform, polyvinyl acetal negative oxygen ion fiber of the present invention, and this manufacture method adopts following steps:
A) getting 8-12 part characterization parameter diameter by mass fraction is 0.1-0.8um, the palygorskite fiber that length is 6-15um; 3-5 part characterization parameter diameter is 0.3-1um, the calcium sulfate crystal whiskers that length is 6-15um, and 4-6 part characterization parameter diameter is 0.5-1um, the Potassium Tetratitanate Whisker that length is 5-15um; After above-mentioned three materials are mixed, at 250-350 DEG C of vacuum kiln roasting 4-6h; Cooling rear by calgon dispersed with stirring in absolute ethyl alcohol, under atmospheric pressure state, carry out Surface Treatment with Plasma 10-20min; Then, cleaning 25-35min loose 60-70 DEG C of deionized water for ultrasonic wavelength-division, gets solution upper strata suspension whisker and removes after filtration the above particle of 16um, and repeat 3-5 time until filtering; After filtering, dry at vacuum drying oven, obtain modified crystal whiskers mixture;
B) get 0.8-1.2 part titanate coupling agent by mass fraction and dilute, be heated to 40-50 DEG C at 1.5-2.5 part alcohol solution; By titanate coupling agent weak solution and steps A) 8-12 part modified crystal whiskers mixture of obtaining stirs 30-45min in mixer under 70-80 DEG C of condition; Dry; Then add nanoscale composition tourmaline powder 8-12 part, EPP bulking agent 1-2 part, surfactant calcium stearate 0.3-0.7 part, airtight stirring reaction 30-45min in mixer under 60-70 DEG C of condition; Add polyvinyl alcohol spin dope 80-120 part, turn/min of 150-200 speed stirs 45-60min, obtains modified polyvinylalcohol spinning solution blend again;
C) by step B) mixing under 90-95 DEG C of constant temperature of modified polyvinylalcohol spinning solution, filtration, the deaeration that obtain, by wet method or dry spinning, acetalization, makes a kind of Spontaneous release negative oxygen ion vinylon.
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 equally numerous embodiment.
Embodiment 1:
The manufacture method of Pioloform, polyvinyl acetal negative oxygen ion fiber of the present invention, the step that this manufacture method adopts is:
A) getting 10 parts of characterization parameter diameters by mass fraction is 0.1-0.8um, the palygorskite fiber that length is 6-15um; 4 parts of characterization parameter diameters are 0.3-1um, the calcium sulfate crystal whiskers that length is 6-15um, and 5 parts of characterization parameter diameters are 0.5-1um, the Potassium Tetratitanate Whisker that length is 5-15um; After above-mentioned three materials are mixed, at 300 DEG C of vacuum kiln roasting 5h; Cooling rear by calgon dispersed with stirring in absolute ethyl alcohol, under atmospheric pressure state, carry out Surface Treatment with Plasma 15min; Then, cleaning 30min loose 65 DEG C of deionized water for ultrasonic wavelength-divisions, gets solution upper strata suspension whisker and removes after filtration the above particle of 16um, and repeat 4 times until filtering; After filtering, dry at vacuum drying oven, obtain modified crystal whiskers mixture;
B) getting 1.0 parts of titanate coupling agents by mass fraction dilutes at 2 parts of alcohol solutions, is heated to 45 DEG C; By titanate coupling agent weak solution and steps A) 10 parts of modified crystal whiskers mixtures obtaining stir 40min in mixer under 75 DEG C of conditions; Dry; Then add 10 parts of nanoscale composition tourmaline powders, 1.5 parts of EPP bulking agents, 0.5 part of surfactant calcium stearate, airtight stirring reaction 40min in mixer under 65 DEG C of conditions; Add 100 parts of polyvinyl alcohol spin dopes, 180 turn/min speed stir 50min, obtain modified polyvinylalcohol spinning solution blend again;
C) by step B) mixing under 92 DEG C of constant temperature of modified polyvinylalcohol spinning solution, filtration, the deaeration that obtain, by wet method or dry spinning, acetalization, makes a kind of Spontaneous release negative oxygen ion vinylon.
Embodiment 2:
The manufacture method of Pioloform, polyvinyl acetal negative oxygen ion fiber of the present invention, this manufacture method adopts following steps:
A) getting 8 parts of characterization parameter diameters by mass fraction is 0.1-0.8um, the palygorskite fiber that length is 6-15um; 3 parts of characterization parameter diameters are 0.3-1um, the calcium sulfate crystal whiskers that length is 6-15um, and 4 parts of characterization parameter diameters are 0.5-1um, the Potassium Tetratitanate Whisker that length is 5-15um; After above-mentioned three materials are mixed, at 250 DEG C of vacuum kiln roasting 4h; Cooling rear by calgon dispersed with stirring in absolute ethyl alcohol, under atmospheric pressure state, carry out Surface Treatment with Plasma 10-20min; Then, cleaning 25min loose 60 DEG C of deionized water for ultrasonic wavelength-divisions, gets solution upper strata suspension whisker and removes after filtration the above particle of 16um, and repeat 3 times until filtering; After filtering, dry at vacuum drying oven, obtain modified crystal whiskers mixture;
B) getting 0.8 part of titanate coupling agent by mass fraction dilutes at 1.5 parts of alcohol solutions, is heated to 40 DEG C; By titanate coupling agent weak solution and steps A) 8 parts of modified crystal whiskers mixtures obtaining stir 30min in mixer under 70 DEG C of conditions; Dry; Then add 8 parts of nanoscale composition tourmaline powders, 1 part of EPP bulking agent, 0.3 part of surfactant calcium stearate, airtight stirring reaction 30min in mixer under 60 DEG C of conditions; Add 80 parts of polyvinyl alcohol spin dopes, 150 turn/min speed stir 45min, obtain modified polyvinylalcohol spinning solution blend again;
C) by step B) mixing under 90 DEG C of constant temperature of modified polyvinylalcohol spinning solution, filtration, the deaeration that obtain, by wet method or dry spinning, acetalization, makes a kind of Spontaneous release negative oxygen ion vinylon.
Embodiment 3:
The manufacture method of Pioloform, polyvinyl acetal negative oxygen ion fiber of the present invention, this manufacture method adopts following steps:
A) getting 12 parts of characterization parameter diameters by mass fraction is 0.1-0.8um, the palygorskite fiber that length is 6-15um; 5 parts of characterization parameter diameters are 0.3-1um, the calcium sulfate crystal whiskers that length is 6-15um, and 6 parts of characterization parameter diameters are 0.5-1um, the Potassium Tetratitanate Whisker that length is 5-15um; After above-mentioned three materials are mixed, at 350 DEG C of vacuum kiln roasting 6h; Cooling rear by calgon dispersed with stirring in absolute ethyl alcohol, under atmospheric pressure state, carry out Surface Treatment with Plasma 20min; Then, cleaning 35min loose 70 DEG C of deionized water for ultrasonic wavelength-divisions, gets solution upper strata suspension whisker and removes after filtration the above particle of 16um, and repeat 5 times until filtering; After filtering, dry at vacuum drying oven, obtain modified crystal whiskers mixture;
B) getting 1.2 parts of titanate coupling agents by mass fraction dilutes at 2.5 parts of alcohol solutions, is heated to 50 DEG C; By titanate coupling agent weak solution and steps A) 12 parts of modified crystal whiskers mixtures obtaining stir 45min in mixer under 80 DEG C of conditions; Dry; Then add 12 parts of nanoscale composition tourmaline powders, 2 parts of EPP bulking agents, 0.7 part of surfactant calcium stearate, airtight stirring reaction 45min in mixer under 70 DEG C of conditions; Add 120 parts of polyvinyl alcohol spin dopes, 200 turn/min speed stir 60min, obtain modified polyvinylalcohol spinning solution blend again;
C) by step B) mixing under 95 DEG C of constant temperature of modified polyvinylalcohol spinning solution, filtration, the deaeration that obtain, by wet method or dry spinning, acetalization, makes a kind of Spontaneous release negative oxygen ion vinylon.
Claims (2)
1. a manufacture method for Pioloform, polyvinyl acetal negative oxygen ion fiber, is characterized in that this manufacture method adopts following steps:
A) getting 8-12 part characterization parameter diameter by mass fraction is 0.1-0.8 μ m, and length is the palygorskite fiber of 6-15 μ m; 3-5 part characterization parameter diameter is 0.3-1 μ m, and length is the calcium sulfate crystal whiskers of 6-15 μ m, and 4-6 part characterization parameter diameter is 0.5-1 μ m, and length is the Potassium Tetratitanate Whisker of 5-15 μ m; After above-mentioned three materials are mixed, at 250-350 DEG C of vacuum kiln roasting 4-6h; Cooling rear by calgon dispersed with stirring in absolute ethyl alcohol, under atmospheric pressure state, carry out Surface Treatment with Plasma 10-20min; Then, cleaning 25-35min loose 60-70 DEG C of deionized water for ultrasonic wavelength-division, 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, dry at vacuum drying oven, obtain modified crystal whiskers mixture;
B) get 0.8-1.2 part titanate coupling agent by mass fraction and dilute, be heated to 40-50 DEG C at 1.5-2.5 part alcohol solution; By titanate coupling agent weak solution and steps A) 8-12 part modified crystal whiskers mixture of obtaining stirs 30-45min in mixer under 70-80 DEG C of condition; Dry; Then add nanoscale composition tourmaline powder 8-12 part, EPP bulking agent 1-2 part, surfactant calcium stearate 0.3-0.7 part, airtight stirring reaction 30-45min in mixer under 60-70 DEG C of condition; Add polyvinyl alcohol spin dope 80-120 part, turn/min of 150-200 speed stirs 45-60min, obtains modified polyvinylalcohol spinning solution blend again;
C) by step B) mixing under 90-95 DEG C of constant temperature of modified polyvinylalcohol spinning solution, filtration, the deaeration that obtain, by wet method or dry spinning, acetalization, makes a kind of Spontaneous release negative oxygen ion vinylon.
2. according to the manufacture method of the Pioloform, polyvinyl acetal negative oxygen ion fiber described in claim 1, it is characterized in that the step that this manufacture method adopts is:
A) getting 10 parts of characterization parameter diameters by mass fraction is 0.1-0.8 μ m, and length is the palygorskite fiber of 6-15 μ m; 4 parts of characterization parameter diameters are 0.3-1 μ m, and length is the calcium sulfate crystal whiskers of 6-15 μ m, and 5 parts of characterization parameter diameters are 0.5-1 μ m, and length is the Potassium Tetratitanate Whisker of 5-15 μ m; After above-mentioned three materials are mixed, at 300 DEG C of vacuum kiln roasting 5h; Cooling rear by calgon dispersed with stirring in absolute ethyl alcohol, under atmospheric pressure state, carry out Surface Treatment with Plasma 15min; Then, cleaning 30min loose 65 DEG C of deionized water for ultrasonic wavelength-divisions, gets solution upper strata suspension whisker and removes after filtration the above particle of 16 μ m, and repeat 4 times until filtering; After filtering, dry at vacuum drying oven, obtain modified crystal whiskers mixture;
B) getting 1.0 parts of titanate coupling agents by mass fraction dilutes at 2 parts of alcohol solutions, is heated to 45 DEG C; By titanate coupling agent weak solution and steps A) 10 parts of modified crystal whiskers mixtures obtaining stir 40min in mixer under 75 DEG C of conditions; Dry; Then add 10 parts of nanoscale composition tourmaline powders, 1.5 parts of EPP bulking agents, 0.5 part of surfactant calcium stearate, airtight stirring reaction 40min in mixer under 65 DEG C of conditions; Add 100 parts of polyvinyl alcohol spin dopes, 180 turn/min speed stir 50min, obtain modified polyvinylalcohol spinning solution blend again;
C) by step B) mixing under 92 DEG C of constant temperature of modified polyvinylalcohol spinning solution, filtration, the deaeration that obtain, by wet method or dry spinning, acetalization, makes a kind of Spontaneous release negative oxygen ion vinylon.
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| CN1483863A (en) * | 2003-07-29 | 2004-03-24 | 东华大学 | Method for preparing whisker material to make modification treatment of spinning chemical fibre |
| CN102134361A (en) * | 2011-05-04 | 2011-07-27 | 刘立文 | Calcium sulfate whisker modified polyvinylalcohol composite material and preparation process thereof |
| CN102337609A (en) * | 2010-07-29 | 2012-02-01 | 上海亿金纳米科技有限公司 | Novel hollow health-care fibers and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1483863A (en) * | 2003-07-29 | 2004-03-24 | 东华大学 | Method for preparing whisker material to make modification treatment of spinning chemical fibre |
| CN102337609A (en) * | 2010-07-29 | 2012-02-01 | 上海亿金纳米科技有限公司 | Novel hollow health-care fibers and preparation method thereof |
| CN102134361A (en) * | 2011-05-04 | 2011-07-27 | 刘立文 | Calcium sulfate whisker modified polyvinylalcohol composite material and preparation process thereof |
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Effective date of registration: 20240607 Address after: Room 207, Building 5, No. 669 Fengtan Road, Xihu District, Hangzhou City, Zhejiang Province, 310030 Patentee after: Hangzhou Oxygen Yiju Environmental Protection Technology Co.,Ltd. Country or region after: China Address before: 310018, No. 2, No. 5, Xiasha Higher Education Park, Hangzhou, Zhejiang Patentee before: ZHEJIANG SCI-TECH University Country or region before: China |