CN109097853B - A kind of preparation method of heatproof, high-intensitive bag-type dusting filter media fibre - Google Patents
A kind of preparation method of heatproof, high-intensitive bag-type dusting filter media fibre Download PDFInfo
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- CN109097853B CN109097853B CN201810933488.1A CN201810933488A CN109097853B CN 109097853 B CN109097853 B CN 109097853B CN 201810933488 A CN201810933488 A CN 201810933488A CN 109097853 B CN109097853 B CN 109097853B
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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
- D01F6/54—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 polymers of unsaturated nitriles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/02—Particle separators, e.g. dust precipitators, having hollow filters made of flexible material
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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Abstract
The invention discloses a kind of heatproofs, the preparation method of high-intensitive bag-type dusting filter media fibre, include the following steps: the pretreatment of (1) polyacrylonitrile powder, the preparation of (2) composite additive, the processing of (3) melt spinning, (4) drawing and setting.Rationally, filter media fibre intensity obtained is high, machinability is good, adsorption filtration effect is strong, the great market competitiveness and application value for the collocation of the method for the present invention technique.
Description
Technical field
The invention belongs to environment-friendly materials technical fields, and in particular to a kind of heatproof, high-intensitive bag-type dusting filter media fibre
Preparation method.
Background technique
The source of air pollution is concentrated mainly on the discharge of the industrial circles such as steel, metallurgy, thermoelectricity, cement and waste incineration
Exhaust gas, these exhaust gas temperature may be up to 300 DEG C or more, even aramid fiber, polyphenylene sulfide (PPS), polyimides, polytetrafluoroethylene (PTFE)
(PTFE) filtering material of contour performance fibers preparation, long-term work under conditions of being also only capable of 200 DEG C or so, high-temperature flue gas is often
It needs just be filtered after increasing the cooling of longer pipe road.Commonly used in the aramid fiber of high temperature filtration, polyphenylene sulfide (PPS),
Polyimides, the contour performance fibers price of polytetrafluoroethylene (PTFE) (PTFE) are generally higher, and current most of iron and steel enterprise is in and is
Maintain yield and lose the state of operation, lack of capital, it is difficult to substantial contribution is put into environmental protection, be faced with interests and environment it
Between difficult selection.
Polyacrylonitrile fibre does not originally have characteristic resistant to high temperature, but excellent polyacrylonitrile fibre is by pre-oxidation, carbon
Change, carbon fiber can be made after graphitization, each step can all generate intermediate product in this process, and preoxidized polyacrylonitrile is fine
Dimension is exactly one of them, and in actual production, a part of pre-oxidized fibers are for continuing deep processing, and other are then only used for making
Make some cheap products, such as sound-proof material, heat-barrier material, fire proofing, forms not little waste.The pre- oxygen of polyacrylonitrile
Chemical fibre dimension limit oxygen index is up to 45% or more, have it is not molten, do not soften, do not shrink, performance is steady in 400 DEG C of atmospheric environment
The features such as determining, cost is relatively low, and pre-oxidized polyacrylonitrile fiber is about 30 yuan/kilogram, and the price of other high-performance fibers is equal
At 120 yuan or so, directly high-temperature flue gas can be filtered, be the ideal chose of high temperature resistant bag-type dusting filtrate.
China's filtering is started late with industrial textile, there is larger gap compared with developed countries, especially in high temperature resistant
In terms of bag-type dusting filtrate, the performance and price of domestic filtering material product, which are all difficult to be formed with external product, to be competed.Polypropylene
Although nitrile pre-oxidized fibers high temperature resistance is excellent, shear strength is poor, and difficulty of processing is larger, in high-temperature bag dust removal filtrate
The application in field still develops slowly, not yet formation industrialized production.It is existing to be used to prepare the poly- of high temperature resistant bag-type dusting filtrate
Acrylonitrile pre-oxidized fibers have the following problems: 1. pre-oxidized polyacrylonitrile fiber self-strengths are lower, and shear strength is poor, adds
Work difficulty is larger, and general acupuncture technique damages it excessive, and product strength is extremely low, is simply possible to use in acoustical cotton, heat insulation foam etc., uncomfortable
For high-temperature bag dust removal field of filter material；2. the Nomex that pre-oxidized polyacrylonitrile fiber is process, surface are slightly made, but internal
Fiber surface it is but very smooth, that there are filter efficiencies in bag dust abatement field is low for this structure, and deashing property is poor, uses
The defects of service life is short need to frequently be replaced, and cost goes up not down.
In order to promote the quality of pre-oxidized polyacrylonitrile fiber, existing method carries out performance improvement enhancing processing to it, such as
Application No. is: 201611114042.3, which disclose a kind of regulation pre-oxidized polyacrylonitrile fiber, homogenizes the method for degree, passes through
Oil removing, boric acid solution immersion modification are first carried out, last pre-oxidation treatment improves the degree that homogenizes of fiber, enhances fiber
Use intensity, stability etc..But such method, which not can solve, promotes pre-oxidized polyacrylonitrile fiber in high temperature resistant
Adaptability application in bag-type dusting field of filter material.
Summary of the invention
The purpose of the present invention is being directed to existing problem, a kind of heatproof, high-intensitive bag-type dusting filter media fibre are provided
Preparation method.
The present invention is achieved by the following technical solutions:
The preparation method of a kind of heatproof, high-intensitive bag-type dusting filter media fibre, includes the following steps:
(1) polyacrylonitrile powder pre-processes:
Potassium permanganate, succinic acid, ionic liquid are subjected to mixing according to 3 ~ 5:1 of weight ratio ~ 2:500 ~ 550 and are put into stirring
In tank, after being stirred continuously 5 ~ 10min of processing, then the polyacrylonitrile powder of 2 ~ 3 times of its gross mass is added into agitator tank, constantly stirs
Mix after 10 ~ 15min of processing mixture A is spare；
(2) prepared by composite additive:
A. multi-walled carbon nanotube, fatty alcohol polyoxyethylene ether, deionized water are carried out according to weight ratio 1:7 ~ 9:100 ~ 110
Mixing is put into agitator tank, and it is spare then to obtain mixed liquid B after 1 ~ 2h of ultrasonic treatment；
B. the resulting mixed liquid B of a will be operated to be poured on Teflon filtration film, then using Suction filtration device 520 ~
It is filtered in the environment of 540kPa and multi-wall carbon nano-tube film is made, manufactured multi wall carbon is received followed in turn by deionized water and methanol
Mitron film carries out repeated flushing, until after cleaning solution is colourless, then temperature is put into multi-wall carbon nano-tube film taking-up and is
It is dried, is taken out after 8 ~ 10h spare in 90 ~ 94 DEG C of vacuum oven；
C. will operation b treated multi-wall carbon nano-tube film is put into progress He ion irradiation processing in irradiation box, it is complete
It is spare at rear taking-up；
D. by Zinc diacetate dihydrate, N, N-dimethylformamide carries out mixing according to weight ratio 1:5 ~ 7 and puts into agitator tank
It is interior, handled with 1200 ~ 1400 revs/min of revolving speed high-speed stirred take out after 40 ~ 50min mixed liquor C is spare；
E. the resulting mixed liquor C of d will be operated to put into reaction kettle, mixed liquor C total volume is then added into reaction kettle
Then 38 ~ 42% dehydrated alcohol is added into reaction kettle again with 600 ~ 700 revs/min of revolving speed 30 ~ 35min of stir process
17 ~ 19% polyvinylpyrrolidone of mixed liquor C gross mass, 19 ~ 22% butyl titanate take out mixed after being ultrasonically treated 2 ~ 2.5h
It is spare to close liquid D；
F. will be in mixed liquor D made from operation c treated multi-wall carbon nano-tube film is immersed in operation e, heating is kept
The temperature of mixed liquor D is 40 ~ 46 DEG C, after constantly 2 ~ 3h of ultrasonic treatment, then high speed centrifugation processing is carried out, then with deionized water pair
It is centrifuged object to rinse one time, finally put it into again in the oxygen-free environment that temperature is 300 ~ 330 DEG C after 3 ~ 5h of heat preservation and dryness processing
It takes out, it is spare to obtain composite additive；
(3) melt spinning is handled:
The resulting mixture A of step (1) and step (2) resulting composite additive are carried out according to weight ratio 100:6 ~ 9
Progress melt spinning processing in twin-screw spinning machine is put into mixing, while being also passed through to the melt zone of twin-screw spinning machine oxygen-containing
Gas, finally it is spare that semi-finished product silk is made in extrusion；
(4) drawing and setting:
Xeothermic stretching is directly carried out to semi-finished product silk made from step (3), the temperature for controlling stretching is 120 ~ 130 DEG C, is drawn
The general times stretched are 5 ~ 6 times, then carry out cleaning cooling to the fiber after stretching with hot water, finally putting it into temperature again is
Thermal finalization is handled in 155 ~ 165 DEG C of hot-air.
Further, ionic liquid as described in step (1) is disubstituted imidazole type ionic liquid.
Further, ultrasonic frequency when ultrasonic treatment described in step (2) operation a is 300 ~ 350kHz.
Further, step (2) operation c described in He ion irradiation processing when control irradiation energy be 330 ~
The temperature control of 350keV, irradiation are 460 ~ 480 DEG C, and injection rate is 2 ~ 4 × 1016 cm-2。
Further, ultrasonic frequency when ultrasonic treatment described in step (2) operation f is 520 ~ 550kHz.
Further, oxygen-containing gas described in step (3) is oxygen, and controlling the flow that it is passed through is 3 ~ 5ml/min.
Further, in twin-screw spinning machine described in step (3) screw speed be 80 ~ 100 revs/min, control into
Expect that section temperature is 174 ~ 178 DEG C, fluxing zone temperature is 188 ~ 192 DEG C, melt zone temperature is 210 ~ 214 DEG C.
Further, the temperature of hot water described in step (4) is 60 ~ 65 DEG C.
The qualities such as the heatproof of pre-oxidized polyacrylonitrile fiber are suitable for the application in high temperature resistant bag-type dusting field of filter material, but
The performances short slab such as intensity, machinability limits its further popularization and use.In this regard, the present invention in view of the foregoing drawbacks problem into
Optimal improvements are gone, final pre-oxidized polyacrylonitrile fiber obtained can be used for the production of high temperature resistant bag-type dusting filtrate well
In.Wherein, oxidation processes first have been carried out to polyacrylonitrile powder raw material with potassium permanganate, succinic acid, can reduced subsequent pre-
The time of oxidation processes and temperature, help going on smoothly for working process, be then prepared for a kind of special composite additive at
Point, the bulk composition of this composite additive is multi-walled carbon nanotube, when preparation, multi-walled carbon nanotube is first processed into multi wall carbon and is received
Mitron film is convenient for subsequent modification, has then carried out the processing of He ion irradiation to multi-wall carbon nano-tube film, this irradiation
Processing etches nanotube walls, so that wall portion grouping knits and deforms, is broken, and texturing tube wall tissue, it is promoted
Whole surface roughness, while also irradiation introduces the helium bubble tissue of small particle, this tissue energy on multi-walled carbon nanotubes
The adsorption capacity of multi-walled carbon nanotube is further promoted, but the certain intensity of multi-walled carbon nanotube can be damaged, is then prepared for again
Mixed liquor D ingredient, the multi-wall carbon nano-tube film after radiation treatment is immersed in wherein, at this time the precursor substance in mixed liquor D
Deposition attachment is carried out under the action of ultrasonic wave, and dehydration finally occurs under subsequent high temperature drying condition and forms one kind by ZnO-
TiO2Compound nano components, this ingredient are enriched in the injury region of multi-walled carbon nanotube, form reinforcement tissue, make up and improve
The intensity of multi-walled carbon nanotube, at the same formation of this tissue more help to enhance multi-walled carbon nanotube ingredient and polyacrylonitrile powder at
The compatible blending divided combines, and finally squeezes out manufactured composite additive and polyacrylonitrile powder blended melting, stretches thermal finalization
After processing, formation be a kind of composite additive filled with a large amount of hollow structures modified polyacrylonitrile pre-oxidized fibers,
Intensity quality is obviously improved, and adsorption capacity is strong, and Nomex is made in use, can not only come by fiber weaving cooperation
Filter absorption, single fiber itself also has good absorption crystallized ability, improves the effect of contamination filtrating, and then improves poly-
Adaptability application of the acrylonitrile pre-oxidized fibers in high temperature resistant bag-type dusting field of filter material.
The present invention has the advantage that compared with prior art
Rationally, filter media fibre intensity obtained is high, machinability is good, adsorption filtration effect for the collocation of the method for the present invention technique
By force, the great market competitiveness and application value.
Specific embodiment
Embodiment 1
The preparation method of a kind of heatproof, high-intensitive bag-type dusting filter media fibre, includes the following steps:
(1) polyacrylonitrile powder pre-processes:
Potassium permanganate, succinic acid, ionic liquid are carried out mixing according to weight ratio 3:1:500 to be put into agitator tank, no
After disconnected stir process 5min, then the polyacrylonitrile powder of 2 times of its gross mass is added into agitator tank, is stirred continuously processing 10min
It is spare that mixture A is obtained afterwards；
(2) prepared by composite additive:
A. multi-walled carbon nanotube, fatty alcohol polyoxyethylene ether, deionized water are subjected to mixing throwing according to weight ratio 1:7:100
Enter into agitator tank, it is spare then to obtain mixed liquid B after ultrasonic treatment 1h；
B. the resulting mixed liquid B of a will be operated to be poured on Teflon filtration film, then existed using Suction filtration device
It is filtered in the environment of 520kPa and multi-wall carbon nano-tube film is made, manufactured multi wall carbon is received followed in turn by deionized water and methanol
Mitron film carries out repeated flushing, until after cleaning solution is colourless, then temperature is put into multi-wall carbon nano-tube film taking-up and is
It is dried, is taken out after 8h spare in 90 DEG C of vacuum oven；
C. will operation b treated multi-wall carbon nano-tube film is put into progress He ion irradiation processing in irradiation box, it is complete
It is spare at rear taking-up；
D. Zinc diacetate dihydrate, n,N dimethylformamide mixing is carried out according to weight ratio 1:5 to put into agitator tank,
Handled with 1200 revs/min of revolving speed high-speed stirred take out after 40min mixed liquor C is spare；
E. the resulting mixed liquor C of d will be operated to put into reaction kettle, mixed liquor C total volume is then added into reaction kettle
Then the total matter of mixed liquor C is added with 600 revs/min of revolving speed stir process 30min in 38% dehydrated alcohol into reaction kettle again
Measure 17% polyvinylpyrrolidone, 19% butyl titanate, be ultrasonically treated 2h after take out mixed liquor D is spare；
F. will be in mixed liquor D made from operation c treated multi-wall carbon nano-tube film is immersed in operation e, heating is kept
The temperature of mixed liquor D is 40 DEG C, after being constantly ultrasonically treated 2h, then high speed centrifugation processing is carried out, then with deionized water to centrifugation
Object rinses one time, finally puts it into heat preservation and dryness in the oxygen-free environment that temperature is 300 DEG C again and takes out after handling 3h, obtains compound
Additive is spare；
(3) melt spinning is handled:
The resulting mixture A of step (1) and step (2) resulting composite additive are mixed according to weight ratio 100:6
Progress melt spinning processing in twin-screw spinning machine is put into conjunction, while being also passed through to the melt zone of twin-screw spinning machine oxygenous
Body, finally it is spare that semi-finished product silk is made in extrusion；
(4) drawing and setting:
Xeothermic stretching is directly carried out to semi-finished product silk made from step (3), the temperature for controlling stretching is 120 DEG C, stretching
General times are 5 times, then carry out cleaning cooling to the fiber after stretching with hot water, and finally putting it into temperature again is 155 DEG C
Hot-air in thermal finalization processing.
Further, ionic liquid as described in step (1) is disubstituted imidazole type ionic liquid.
Further, ultrasonic frequency when ultrasonic treatment described in step (2) operation a is 300kHz.
Further, the energy of control irradiation is 330keV when the processing of He ion irradiation described in step (2) operation c,
The temperature control of irradiation is 460 DEG C, and injection rate is 2 × 1016 cm-2。
Further, ultrasonic frequency when ultrasonic treatment described in step (2) operation f is 520kHz.
Further, oxygen-containing gas described in step (3) is oxygen, and controlling the flow that it is passed through is 3ml/min.
Further, screw speed is 80 revs/min in twin-screw spinning machine described in step (3), controls feed zone
Temperature is 174 DEG C, fluxing zone temperature is 188 DEG C, melt zone temperature is 210 DEG C.
Further, the temperature of hot water described in step (4) is 60 DEG C.
Embodiment 2
The preparation method of a kind of heatproof, high-intensitive bag-type dusting filter media fibre, includes the following steps:
(1) polyacrylonitrile powder pre-processes:
Potassium permanganate, succinic acid, ionic liquid are carried out mixing according to weight ratio 4:1.5:530 to be put into agitator tank,
It is stirred continuously after handling 8min, then the polyacrylonitrile powder of 2.5 times of its gross mass is added into agitator tank, be stirred continuously processing
It is spare that mixture A is obtained after 13min；
(2) prepared by composite additive:
A. multi-walled carbon nanotube, fatty alcohol polyoxyethylene ether, deionized water are subjected to mixing throwing according to weight ratio 1:8:105
Enter into agitator tank, it is spare then to obtain mixed liquid B after ultrasonic treatment 1.5h；
B. the resulting mixed liquid B of a will be operated to be poured on Teflon filtration film, then existed using Suction filtration device
It is filtered in the environment of 530kPa and multi-wall carbon nano-tube film is made, manufactured multi wall carbon is received followed in turn by deionized water and methanol
Mitron film carries out repeated flushing, until after cleaning solution is colourless, then temperature is put into multi-wall carbon nano-tube film taking-up and is
It is dried, is taken out after 9h spare in 92 DEG C of vacuum oven；
C. will operation b treated multi-wall carbon nano-tube film is put into progress He ion irradiation processing in irradiation box, it is complete
It is spare at rear taking-up；
D. Zinc diacetate dihydrate, n,N dimethylformamide mixing is carried out according to weight ratio 1:6 to put into agitator tank,
Handled with 1300 revs/min of revolving speed high-speed stirred take out after 45min mixed liquor C is spare；
E. the resulting mixed liquor C of d will be operated to put into reaction kettle, mixed liquor C total volume is then added into reaction kettle
Then the total matter of mixed liquor C is added with 650 revs/min of revolving speed stir process 33min in 40% dehydrated alcohol into reaction kettle again
Measure 18% polyvinylpyrrolidone, 21% butyl titanate, be ultrasonically treated 2.3h after take out mixed liquor D is spare；
F. will be in mixed liquor D made from operation c treated multi-wall carbon nano-tube film is immersed in operation e, heating is kept
The temperature of mixed liquor D is 43 DEG C, after being constantly ultrasonically treated 2.5h, then carries out high speed centrifugation processing, then with deionized water to from
Heart object rinses one time, finally puts it into heat preservation and dryness in the oxygen-free environment that temperature is 320 DEG C again and takes out after handling 4h, must answer
It is spare to close additive；
(3) melt spinning is handled:
The resulting mixture A of step (1) and step (2) resulting composite additive are mixed according to weight ratio 100:8
Progress melt spinning processing in twin-screw spinning machine is put into conjunction, while being also passed through to the melt zone of twin-screw spinning machine oxygenous
Body, finally it is spare that semi-finished product silk is made in extrusion；
(4) drawing and setting:
Xeothermic stretching is directly carried out to semi-finished product silk made from step (3), the temperature for controlling stretching is 125 DEG C, stretching
General times are 5.5 times, then carry out cleaning cooling to the fiber after stretching with hot water, and finally putting it into temperature again is 160
DEG C hot-air in thermal finalization processing.
Further, ionic liquid as described in step (1) is disubstituted imidazole type ionic liquid.
Further, ultrasonic frequency when ultrasonic treatment described in step (2) operation a is 330kHz.
Further, the energy of control irradiation is 340keV when the processing of He ion irradiation described in step (2) operation c,
The temperature control of irradiation is 470 DEG C, and injection rate is 3 × 1016 cm-2。
Further, ultrasonic frequency when ultrasonic treatment described in step (2) operation f is 540kHz.
Further, oxygen-containing gas described in step (3) is oxygen, and controlling the flow that it is passed through is 4ml/min.
Further, screw speed is 90 revs/min in twin-screw spinning machine described in step (3), controls feed zone
Temperature is 176 DEG C, fluxing zone temperature is 190 DEG C, melt zone temperature is 212 DEG C.
Further, the temperature of hot water described in step (4) is 63 DEG C.
Embodiment 3
The preparation method of a kind of heatproof, high-intensitive bag-type dusting filter media fibre, includes the following steps:
(1) polyacrylonitrile powder pre-processes:
Potassium permanganate, succinic acid, ionic liquid are carried out mixing according to weight ratio 5:2:550 to be put into agitator tank, no
After disconnected stir process 10min, then the polyacrylonitrile powder of 3 times of its gross mass is added into agitator tank, is stirred continuously processing 15min
It is spare that mixture A is obtained afterwards；
(2) prepared by composite additive:
A. multi-walled carbon nanotube, fatty alcohol polyoxyethylene ether, deionized water are subjected to mixing throwing according to weight ratio 1:9:110
Enter into agitator tank, it is spare then to obtain mixed liquid B after ultrasonic treatment 2h；
B. the resulting mixed liquid B of a will be operated to be poured on Teflon filtration film, then existed using Suction filtration device
It is filtered in the environment of 540kPa and multi-wall carbon nano-tube film is made, manufactured multi wall carbon is received followed in turn by deionized water and methanol
Mitron film carries out repeated flushing, until after cleaning solution is colourless, then temperature is put into multi-wall carbon nano-tube film taking-up and is
It is dried, is taken out after 10h spare in 94 DEG C of vacuum oven；
C. will operation b treated multi-wall carbon nano-tube film is put into progress He ion irradiation processing in irradiation box, it is complete
It is spare at rear taking-up；
D. Zinc diacetate dihydrate, n,N dimethylformamide mixing is carried out according to weight ratio 1:7 to put into agitator tank,
Handled with 1400 revs/min of revolving speed high-speed stirred take out after 50min mixed liquor C is spare；
E. the resulting mixed liquor C of d will be operated to put into reaction kettle, mixed liquor C total volume is then added into reaction kettle
Then the total matter of mixed liquor C is added with 700 revs/min of revolving speed stir process 35min in 42% dehydrated alcohol into reaction kettle again
Measure 19% polyvinylpyrrolidone, 22% butyl titanate, be ultrasonically treated 2.5h after take out mixed liquor D is spare；
F. will be in mixed liquor D made from operation c treated multi-wall carbon nano-tube film is immersed in operation e, heating is kept
The temperature of mixed liquor D is 46 DEG C, after being constantly ultrasonically treated 3h, then high speed centrifugation processing is carried out, then with deionized water to centrifugation
Object rinses one time, finally puts it into heat preservation and dryness in the oxygen-free environment that temperature is 330 DEG C again and takes out after handling 5h, obtains compound
Additive is spare；
(3) melt spinning is handled:
The resulting mixture A of step (1) and step (2) resulting composite additive are mixed according to weight ratio 100:9
Progress melt spinning processing in twin-screw spinning machine is put into conjunction, while being also passed through to the melt zone of twin-screw spinning machine oxygenous
Body, finally it is spare that semi-finished product silk is made in extrusion；
(4) drawing and setting:
Xeothermic stretching is directly carried out to semi-finished product silk made from step (3), the temperature for controlling stretching is 130 DEG C, stretching
General times are 6 times, then carry out cleaning cooling to the fiber after stretching with hot water, and finally putting it into temperature again is 165 DEG C
Hot-air in thermal finalization processing.
Further, ionic liquid as described in step (1) is disubstituted imidazole type ionic liquid.
Further, ultrasonic frequency when ultrasonic treatment described in step (2) operation a is 350kHz.
Further, the energy of control irradiation is 350keV when the processing of He ion irradiation described in step (2) operation c,
The temperature control of irradiation is 480 DEG C, and injection rate is 4 × 1016 cm-2。
Further, ultrasonic frequency when ultrasonic treatment described in step (2) operation f is 550kHz.
Further, oxygen-containing gas described in step (3) is oxygen, and controlling the flow that it is passed through is 5ml/min.
Further, screw speed is 100 revs/min in twin-screw spinning machine described in step (3), controls feed zone
Temperature is 178 DEG C, fluxing zone temperature is 192 DEG C, melt zone temperature is 214 DEG C.
Further, the temperature of hot water described in step (4) is 65 DEG C.
Comparative example 1
This comparative example 1 compared with Example 2, in the preparation of step (2) composite additive, eliminates the place of operation c
Reason, method and step in addition to this are all the same.
Comparative example 2
This comparative example 2 compared with Example 2, in the preparation of step (2) composite additive, eliminates operation d, operation
E and subsequent corresponding processing, method and step in addition to this are all the same.
Comparative example 3
This comparative example 3 compared with Example 2, step (3) melt spinning processing in, with etc. mass parts it is commercially available more
The resulting composite additive ingredient of wall carbon nano tube step of replacing (2), method and step in addition to this are all the same.
Comparative example 4
This comparative example 4 compared with Example 2, in the processing of step (3) melt spinning, eliminates obtained by step (2)
Composite additive ingredient addition processing, method and step in addition to this is all the same.
Control group
It homogenizes the side of degree application No. is a kind of: regulation pre-oxidized polyacrylonitrile fiber disclosed in 201611114042.3
Method.
In order to compare effect of the present invention, to above-described embodiment 2, comparative example 1, comparative example 2, comparative example 3,
The corresponding filter media fibre obtained of comparative example 4, control group is tested for the property, and specific correlation data is as shown in table 1 below:
Table 1
Note: fibre strength described in upper table 1 is tested referring to GB/T 3916-1997；The Nomex intensity is
Pre-oxidized polyacrylonitrile fiber and polyphenylene sulfide fibre are subjected to mixing weaving according to weight ratio 60:40, it is woven with low close aramid fiber
Object is base fabric, is made up of identical needle point method technique, and each group is in addition to pre-oxidized polyacrylonitrile fiber type is different, remaining technique
Method is identical；Nomex loss of strength rate is to be put in Nomex obtained under 300 DEG C of environment to keep the temperature at described 300 DEG C
The loss of strength rate measured after processing 12h；The dust-cleaning efficiency is the stripping of the 30 1000Pa cleaning cycle dust measured
From rate.
The synthesis of the filter media fibre made from the method for the present invention it can be seen from upper table 1 has obtained significantly mentioning using quality
It rises, the great market competitiveness and application value.
Claims (8)
1. the preparation method of a kind of heatproof, high-intensitive bag-type dusting filter media fibre, which comprises the steps of:
(1) polyacrylonitrile powder pre-processes:
Potassium permanganate, succinic acid, ionic liquid are subjected to mixing according to 3 ~ 5:1 of weight ratio ~ 2:500 ~ 550 and are put into agitator tank
It is interior, after being stirred continuously 5 ~ 10min of processing, then the polyacrylonitrile powder of 2 ~ 3 times of its gross mass is added into agitator tank, is stirred continuously
It is spare that mixture A is obtained after 10 ~ 15min of processing；
(2) prepared by composite additive:
A. multi-walled carbon nanotube, fatty alcohol polyoxyethylene ether, deionized water are mixed according to weight ratio 1:7 ~ 9:100 ~ 110
It puts into agitator tank, it is spare then to obtain mixed liquid B after 1 ~ 2h of ultrasonic treatment；
B. the resulting mixed liquid B of a will be operated to be poured on Teflon filtration film, then using Suction filtration device 520 ~
It is filtered in the environment of 540kPa and multi-wall carbon nano-tube film is made, manufactured multi wall carbon is received followed in turn by deionized water and methanol
Mitron film carries out repeated flushing, until after cleaning solution is colourless, then temperature is put into multi-wall carbon nano-tube film taking-up and is
It is dried, is taken out after 8 ~ 10h spare in 90 ~ 94 DEG C of vacuum oven；
C. will operation b treated multi-wall carbon nano-tube film is put into progress He ion irradiation processing in irradiation box, after the completion
It takes out spare；
D. Zinc diacetate dihydrate, n,N dimethylformamide mixing is carried out according to weight ratio 1:5 ~ 7 to put into agitator tank, with
1200 ~ 1400 revs/min of revolving speed high-speed stirred handle take out after 40 ~ 50min mixed liquor C is spare；
E. the resulting mixed liquor C of d will be operated to put into reaction kettle, then into reaction kettle be added mixed liquor C total volume 38 ~
Then mixing is added with 600 ~ 700 revs/min of revolving speed 30 ~ 35min of stir process in 42% dehydrated alcohol into reaction kettle again
17 ~ 19% polyvinylpyrrolidone of liquid C gross mass, 19 ~ 22% butyl titanate take out to obtain mixed liquor after being ultrasonically treated 2 ~ 2.5h
D is spare；
F. will be in mixed liquor D made from operation c treated multi-wall carbon nano-tube film is immersed in operation e, heating keeps mixing
The temperature of liquid D is 40 ~ 46 DEG C, after constantly 2 ~ 3h of ultrasonic treatment, then high speed centrifugation processing is carried out, then with deionized water to centrifugation
Object rinses one time, finally puts it into heat preservation and dryness in the oxygen-free environment that temperature is 300 ~ 330 DEG C again and takes out after handling 3 ~ 5h,
It is spare to obtain composite additive；
(3) melt spinning is handled:
The resulting mixture A of step (1) and step (2) resulting composite additive are mixed according to weight ratio 100:6 ~ 9
Progress melt spinning processing in twin-screw spinning machine is put into, while being also passed through to the melt zone of twin-screw spinning machine oxygenous
Body, finally it is spare that semi-finished product silk is made in extrusion；
(4) drawing and setting:
Xeothermic stretching is directly carried out to semi-finished product silk made from step (3), the temperature for controlling stretching is 120 ~ 130 DEG C, stretching
General times be 5 ~ 6 times, cleaning cooling then is carried out to the fiber after stretching with hot water, finally put it into again temperature be 155 ~
Thermal finalization is handled in 165 DEG C of hot-air.
2. the preparation method of a kind of heatproof according to claim 1, high-intensitive bag-type dusting filter media fibre, feature exist
In ionic liquid as described in step (1) is disubstituted imidazole type ionic liquid.
3. the preparation method of a kind of heatproof according to claim 1, high-intensitive bag-type dusting filter media fibre, feature exist
In ultrasonic frequency when step (2) operates ultrasonic treatment described in a is 300 ~ 350kHz.
4. the preparation method of a kind of heatproof according to claim 1, high-intensitive bag-type dusting filter media fibre, feature exist
In the energy of control irradiation is 330 ~ 350keV, the temperature of irradiation when step (2) operates the processing of He ion irradiation described in c
Control is 460 ~ 480 DEG C, and injection rate is 2 ~ 4 × 1016 cm-2。
5. the preparation method of a kind of heatproof according to claim 1, high-intensitive bag-type dusting filter media fibre, feature exist
In ultrasonic frequency when step (2) operates ultrasonic treatment described in f is 520 ~ 550kHz.
6. the preparation method of a kind of heatproof according to claim 1, high-intensitive bag-type dusting filter media fibre, feature exist
In oxygen-containing gas described in step (3) is oxygen, and controlling the flow that it is passed through is 3 ~ 5ml/min.
7. the preparation method of a kind of heatproof according to claim 1, high-intensitive bag-type dusting filter media fibre, feature exist
In, in twin-screw spinning machine described in step (3) screw speed be 80 ~ 100 revs/min, control feed zone temperature be 174 ~
178 DEG C, fluxing zone temperature be 188 ~ 192 DEG C, melt zone temperature is 210 ~ 214 DEG C.
8. the preparation method of a kind of heatproof according to claim 1, high-intensitive bag-type dusting filter media fibre, feature exist
In the temperature of hot water described in step (4) is 60 ~ 65 DEG C.
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