CN1137000C - Ion exchange fibre and its preparing process - Google Patents

Ion exchange fibre and its preparing process Download PDF

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Publication number
CN1137000C
CN1137000C CNB021252041A CN02125204A CN1137000C CN 1137000 C CN1137000 C CN 1137000C CN B021252041 A CNB021252041 A CN B021252041A CN 02125204 A CN02125204 A CN 02125204A CN 1137000 C CN1137000 C CN 1137000C
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fiber
core
ion
skin
exchange fibre
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CN1396001A (en
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鲁 齐
齐鲁
叶建忠
邹建柱
李和玉
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China Petroleum and Chemical Corp
Tianjin Polytechnic University
China Petrochemical Corp
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China Petroleum and Chemical Corp
Tianjin Polytechnic University
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Abstract

The present invention relates to an ion exchange fiber and a manufacturing method thereof. A fiber is characterized in that the fiber is provided with a skin-core structure, and the weight ratio of a skin core is from 3: 7 to 7: 3; skin layer materials comprise the components of the following proportion: 20 to 80% of polystyrene with high impact resistance, 19.5 to 79.9% of polystyrene and 0.5 to 0.1% of cross-linking agents; a core layer material comprises the components of the following proportion: 10 to 30% of polystyrene with high impact resistance, 60.6 to 74.4% of polypropylene, 5 to 15% of polyethylene, 4 to 0.5% of compatibilizer and 0.4 to 0.1% of the cross-linking agents. The manufacturing method is characterized in that 1. in a skin layer material manufacturing process, after the skin layer materials are uniformly mixed according to the components of the proportion, the skin layer materials are extruded by two screws through granulation at the temperature of 220 to 260 DEG C, and the skin layer materials are manufactured; 2. in a core layer material manufacturing process, the core layer material is manufactured in the method which is similar to the method one; 3. in a composite wire manufacturing process, the manufactured skin materials and the manufactured core materials are spun in proportion and are made into a winding wire which is stretched by 1.5 to 3 times at the temperature of 90 to 110 DEG C; 4. in a fiber cross-linking process, the composite wire is put into a cross-linking solution prepared from paraformaldehyde, glacial acetic acid and concentrated sulfuric acid according to the proportion of 8-2 to 25-31 to 67, and reacts for 1.5 to 3 hours at the temperature of 80 to 95 DEG C; 5. in a fiber functionalized processing process, the obtained cross-linking fibers react in a functionalization mode according to requirements. Thus, a corresponding ion exchange fiber can be obtained.

Description

A kind of ion-exchange fibre and manufacture method thereof
(1) technical field
The present invention relates to chemical fibre material and manufacture method technology thereof, be specially a kind of ion-exchange fibre and manufacture method technology thereof.Its IPC Main classification number plan is Int.Cl7B01G 39/20.
(2) background technology
The present invention relates to a kind of ion-exchange fibre and manufacture method thereof.Ion-exchange fibre is a kind of fibrous ion exchanger, compare with ion exchange resin to have thinner straight warp, very big specific surface, exchange and elution speed faster, can the various forms application etc. advantage.Therefore range of application constantly enlarges.
The Japan Patent spy opens the manufacture method that clear 63-108039 has reported a kind of ion-exchange fibre.This fiber is to be sea component with the polystyrene, is island component with the polypropylene, carries out melt spinning under 250 ℃ and 260 ℃, and the island number is 16.This manufacture method relates to composite spinning technology, and its deficiency is to need to use the bigger fabric of island-in-sea type filament spinning component of manufacture difficulty; The 2nd, though it adopts the island pattern, and uses the polypropylene fortifying fibre, owing to do not solve the problem of phase separation between sea and the island polymer, thus make the fiber after the functionalization have necessarily degree of peeling off.Up-to-date Chinese patent CN discloses a kind of polystyrene and polyolefinic blend for 1279135A number through general apparatus for melt spinning manufacturing " multicore fabric of island-in-sea type blending type ion-exchange fibre " manufacture method.Though this kind method has used general apparatus for melt spinning to make the blending type ion-exchange fibre, but there is the problem of phase separation between polystyrene and polyolefin two base polymers equally in this method, its intensity is very low after the fiber functionalization, and service life is short, is unfavorable for practical application.
(3) technology contents
At the deficiencies in the prior art, the quasi-solution of the present invention phase detachment technique problem between the polymer that described fabric of island-in-sea type or blending type ion-exchange fibre all exist of determining, a kind of simpler is provided, but compatibility is better between the polymer, service life is long ion-exchange fibre and manufacture method technology thereof.
The technical scheme that the present invention solve the technical problem is: design a kind of ion-exchange fibre, it is characterized in that this fiber has core-sheath composite structure, the core-skin weight ratio is 3: 7-7: 3; The percentage by weight prescription of its cortex material is:
High impact polystyrene 20-80%,
Polystyrene 19.5-79.9%,
Crosslinking agent 0.5-0.1%;
The percentage by weight prescription of its core layer material is:
High impact polystyrene 10-30%,
Polypropylene 60.6-74.4%,
Polyethylene 5-15%,
Bulking agent 4-0.5%,
Crosslinking agent 0.4-0.1%;
Wherein, the melt index of high impact polystyrene is 4-30, and the melt index of polystyrene is 5-50, and polyacrylic melt index is 18-50, and poly melt index is 15-60; Described crosslinking agent is 2,5-dimethyl-2, two (tert-butyl peroxy base) hexanes (AD), 2 of 5-, 5-dimethyl-2, two (tert-butyl peroxy base) hexins-3 (YD) of 5-, α, one or more in α-(tert-butyl peroxy base) diisopropylbenzene (DIPB), the cumyl peroxide (DCP); Used crosslinker solution is paraformaldehyde, glacial acetic acid, the concentrated sulfuric acid in 8-2 in the fiber cross-linking process: 2 5-31: the crosslinker solution of 67 ratios preparation.
Ion-exchange fibre of the present invention adopts core-skin composite spinning silk method spinning, and its process is as follows:
1. make the fiber sheath layered material: after high impact styrene, polystyrene, the crosslinking agent of will fill a prescription described melt index and ratio mixes, extrude through twin-screw under 220-260 ℃, granulation produces the fiber sheath layered material;
2. make the fibre core layered material: after high impact polystyrene, polypropylene, polyethylene, bulking agent, the crosslinking agent of will fill a prescription described melt index and ratio mixes, extrude through twin-screw under 180-230 ℃, granulation produces the fibre core layered material;
3. make the core-skin composite filament: above-mentioned 1,2 described cortex materials and core layer material are spun out undrawn yarn with core-skin composite spinning silk machine; Undrawn yarn is stretched under 90-110 ℃ of temperature, draw ratio 1.5-3 doubly promptly obtains the core-skin composite filament again;
4. fiber cross-linking reaction: gained core-skin composite filament put into contain paraformaldehyde, glacial acetic acid, the concentrated sulfuric acid in 8-2: 25-31: the crosslinker solution of 67 ratios preparation 80-95 ℃ of reaction 1.5-3 hour down, obtains cross filament;
5. fiber functionalization: as required, the gained cross filament is carried out reaction kinetic, can obtain corresponding ion-exchange fibre.
After tested, the exchange capacity of gained fiber is that the phenomenon of phase separation between the core-skin layer of 1.8-3.8mmol/g, particularly resultant ion-exchange fibre is greatly improved, and practicality strengthens, and service life is reinforcement greatly also.
(4) specific embodiment
Ion-exchange fibre of the present invention has core-sheath composite structure, and the core-skin weight ratio is 3: 7-7: 3; The percentage by weight prescription of its cortex material is:
High impact polystyrene 20-80%,
Polystyrene 19.5-79.9%,
Crosslinking agent 0.5-0.1%;
The percentage by weight prescription of its core layer material is:
High impact polystyrene 10-30%,
Polypropylene 60.6-74.4%,
Polyethylene 5-15%,
Bulking agent 4-0.5%,
Crosslinking agent 0.4-0.1%;
Wherein, the melt index of high impact polystyrene is 4-30, and the melt index of polystyrene is 5-50, and polyacrylic melt index is 18-50, and poly melt index is 15-60; Described crosslinking agent is 2,5-dimethyl-2, two (tert-butyl peroxy base) hexanes (AD), 2 of 5-, 5-dimethyl-2, two (tert-butyl peroxy base) hexins-3 (YD) of 5-, α, one or more in α-(tert-butyl peroxy base) diisopropylbenzene (DIPB), the cumyl peroxide (DCP); Used crosslinker solution is paraformaldehyde, glacial acetic acid, the concentrated sulfuric acid in 8-2: 25-31 in the fiber cross-linking process: the crosslinker solution of 67 ratios preparation.
All design the high impact polystyrene that has used described ratio in the cortex material of ion-exchange fibre of the present invention and the prescription of core layer material, use its objective is in order to increase the compatibility between the polymer, and can produce certain crosslinked action, can solve the problem of phase separation between polystyrene and polyolefin two base polymers preferably.
In order further to improve the compatibility between the polymer, ion-exchange fibre of the present invention has added bulking agent in the core layer material of fiber.Described bulking agent be SB (styrene. butadiene block copolymer), SBS (styrene. butadiene. styrene block copolymer), SBSBS (styrene. butadiene. styrene. butadiene. styrene block copolymer) in a kind of.
In order to increase the adhesion between skin, core material inside and skin, the core material interfacial polymerization thing, solve the problem of phase separation between polystyrene and polyolefin two base polymers better, ion-exchange fibre of the present invention has all added the crosslinking agent of proper proportion in the skin of fiber, core layer material.Described crosslinking agent is 2,5-dimethyl-2, two (tert-butyl peroxy base) hexanes (AD), 2 of 5-, 5-dimethyl-2, two (tert-butyl peroxy base) hexins-3 (YD) of 5-, α, one or more in α-(tert-butyl peroxy base) diisopropylbenzene (DIPB), the cumyl peroxide (DCP).
Ion-exchange fibre of the present invention has core-sheath composite structure, and the core-skin weight ratio is 3: 7-7: 3, but even more ideal be 4: 6-6: 4.
The manufacture method of ion-exchange fibre of the present invention is simply said so: the special-purpose spinning material of making skin, two kinds of ion-exchange fibres of core by the prescription requirement respectively, general core-skin composite spinning silk assembly is made core-skin composite fiber in composite spinning equipment, composite fibre is stretched, crosslinked, sulfonation or aminating reaction again.Sulfonation can make the strong-acid type ion-exchange fibre; Fiber after crosslinked is carried out chloromethylation, can make strong base or weak base type ion-exchange fibre through different aminations.
The manufacture method of ion-exchange fibre of the present invention is to adopt core-skin composite spinning silk method spinning ion-exchange fibre, is specifically: by the prescription requirement
1. make the fiber sheath layered material: with melt index is the 20-80% that the high impact styrene of 4-30 accounts for compound weight, and melt index is the polystyrene of 5-50, accounts for 19.5-79.9%, crosslinking agent 0.1-0.5%, after mixing by weight percentage, under 220-260 ℃, extrude granulation through twin-screw.Produce the ion-exchange fibre cortex material;
2. make the fibre core layered material: the polypropylene that with melt index is 18-50 is the polyethylene of 15-60 accounts for compound weight by 5-15%, high impact polystyrene 10-35% by 50.6-84.4%, melt index, bulking agent accounts for 0.5-4%, after crosslinking agent accounts for the percentage by weight mixing of 0.1-0.4%, under 180-230 ℃, extrude granulation through twin-screw.Produce the ion-exchange fibre core layer material;
3. make the core-skin composite filament: above-mentioned 1,2 two kind of pelletizing material are spun out undrawn yarn with core-skin composite spinning silk machine; Again with undrawn yarn through 90-110 ℃, the stretching of draw ratio 1.5-3 obtains the core-skin composite filament;
4. fiber is crosslinked: the core-skin composite filament is put into contained paraformaldehyde, glacial acetic acid, the concentrated sulfuric acid in 2-8: 25-35: the crosslinker solution of 57-73 ratio preparation 80-95 ℃ of reaction 1.5-3 hour down, obtains cross filament;
5. fiber functionalization: as required, the gained cross filament is carried out reaction kinetic, can obtain corresponding ion-exchange fibre.
In described the 5th step of ion-exchange fibre manufacture method of the present invention, promptly in " 5. fiber functionalization " technology, as required, can carry out fiber sulfonation treatment process or amination treatment technology.When carrying out fiber sulfonation treatment process, can obtain the strong-acid type ion-exchange fibre.Concrete fiber sulfonation treatment process is: the cross filament of the 4th step gained is immersed dichloroethanes and the concentrated sulfuric acid in 8-2: in the sulfonated liquid that the 92-98 ratio is prepared, reacted 2-3 hour down at 70-80 ℃, rise to 90-98 ℃ then, reacted 2-3 hour, and can obtain described strong-acid type ion-exchange fibre.
When carrying out fiber amination treatment technology, can obtain alkali type ion-exchange fibre.When carrying out the strong amination treatment technology of fiber, can obtain the strong base ion-exchange fibre; A little less than carrying out fiber, during amination treatment technology, can obtain weak base type ion-exchange fibre.Described strong amination treatment technology is specifically: the cross filament of the 4th step gained immersed contain in the chloromethyl ether solution of catalyst, 45 ℃ down reaction obtain the chloromethylation fiber after 8-10 hour; Again the gained fiber is put into trimethylamine solution, at room temperature react 20-24 after individual hour, promptly obtain the strong base ion-exchange fibre; Amination treatment technology specifically a little less than described: the immersion of gained cross filament is contained in the chloromethyl ether solution of catalyst, obtain the chloromethylation fiber in reaction under 45 ℃ after 8-10 hour; Again the gained fiber is put into ethylenediamine solution, promptly obtain weak base type ion-exchange fibre after 12-15 hour in reaction under 50 ℃.
After measured, the exchange capacity of ion-exchange fibre of the present invention is 1.8-3.8mmol/g, and particularly the core-skin layer phenomenon of phase separation of gained ion-exchange fibre is greatly improved long service life.
Below provide several specific embodiment of the present invention:
Embodiment 1:
1. get melt index and be 20 parts of 30 high impact styrenes, melt index is 79.9 parts of 50 polystyrene, crosslinking agent 2,5-dimethyl-2,0.1 part of two (tert-butyl peroxy base) hexane (AD) of 5-, mix after twin-screw, under 210 ℃ of temperature, extrude, granulation, prepare the ion-exchange fibre cortex material;
2. get melt index and be 18 polypropylene by 74.4 parts, melt index be 15 polyethylene be 15 parts, high impact polystyrene be 10 parts, bulking agent SB (styrene. butadiene block copolymer) account for 0.5 part, crosslinking agent 2,5-dimethyl-2, two (tert-butyl peroxy base) hexanes (AD) of 5-account for 0.1 part, after the mixing, under 230 ℃ through twin-screw extrude, granulation, prepare the ion-exchange fibre core layer material;
With above-mentioned 1,2 two kind of section through core-skin composite spinning silk machine, with 7: 3 core-skin ratios, under 260 ℃, spin out undrawn yarn, undrawn yarn is after washing, in 100 ℃ of following 3 times of stretching, oven dry, cut-out obtains the core-skin composite short fiber;
4. 2 parts of paraformaldehydes, 35 parts of glacial acetic acid, 63 parts of dense stream acid are mixed, make crosslinker solution, will obtain the core-skin composite short fiber and put into this mixed liquor, be heated to 80 ℃, reacted 3 hours, obtain cross filament;
5. cross filament is immersed and contain dichloroethanes,, rise to 95 ℃ then, reacted 3 hours, can obtain described ion-exchange fibre 80 ℃ of reactions 3 hours down by in 2 parts, the sulfonation solution of 98 parts of preparations of the concentrated sulfuric acid.After tested, the exchange capacity of fiber is 3.8mmol/g, and the fiber phenomenon of phase separation is greatly improved.
Embodiment 2:
1. get melt index and be 80 parts of 10 high impact styrenes, melt index is 19.5 parts of 5 polystyrene, crosslinking agent 2,5-dimethyl-2, two (tert-butyl peroxy base) hexins-3 (YD) of 5-, 0.5 part, mix after twin-screw, under 230 ℃ of temperature, extrude, granulation, prepare the fiber sheath layered material;
2. getting melt index and be 45 polypropylene is that 40 polyethylene is that 5 parts, high impact polystyrene are 30 parts by 60.7 parts, melt index, bulking agent SBS (styrene. butadiene. styrene block copolymer) account for 4 parts, crosslinking agent 2,5-dimethyl-2, two (tert-butyl peroxy base) hexins-3 (YD) of 5-account for 0.4 part, after the mixing, extrude through twin-screw under 180 ℃, the fibre core layered material is prepared in granulation;
3. above-mentioned two kinds of sections are spun out undrawn yarn through core-skin composite spinning silk machine by 3: 7 core-skin weight ratios under 280 ℃; Undrawn yarn after 100 ℃ of following 3 times of stretchings, oven dry, cutting off, obtains the core-skin composite short fiber after washing;
4. 8 parts of paraformaldehydes, 25 parts of glacial acetic acid, 67 parts of dense stream acid are mixed, will obtain the core-skin composite short fiber and put into this crosslinker solution, be heated to 95 ℃, reacted 1.5 hours, obtain cross filament.
5. cross filament is immersed and contain dichloroethanes,, rise to 98 ℃ then, reacted 2 hours, obtain described ion-exchange fibre 80 ℃ of reactions 3 hours down by in 2 parts, the sulfonation solution of 98 parts of preparations of the concentrated sulfuric acid.After tested, the exchange capacity of this fiber is 1.6mmol/g, and the fiber phenomenon of phase separation is greatly improved.
Embodiment 3:
1. get melt index and be 50 parts of 4 high impact styrenes, melt index is 49.6 parts of 10 polystyrene, crosslinking agent α, α-(tert-butyl peroxy base) diisopropylbenzene (DIPB), 0.4 part, after the mixing, through twin-screw, under 240 ℃ of temperature, extrude, granulation, prepare the fiber sheath layered material;
2. getting melt index and be 25 polypropylene is that 25 polyethylene is that 10 parts, high impact polystyrene are 25 parts by 62.8 parts, melt index, bulking agent SBSBS (styrene. butadiene. styrene. butadiene. styrene block copolymer) account for 2 parts, crosslinking agent α, α-(tert-butyl peroxy base) diisopropylbenzene (DIPB) accounts for 0.2 part, after the mixing, extrude through twin-screw under 190 ℃, the fibre core layered material is prepared in granulation;
With above-mentioned two kinds of sections through core-skin composite spinning silk machine, with 6: 4 core-skin ratios, under 270 ℃, spin out undrawn yarn, undrawn yarn obtains the core-skin composite short fiber after 100 ℃ of following 3 times of stretching, oven dry, cut-out after washing;
4. 5 parts of paraformaldehydes, 30 parts of glacial acetic acid, 65 parts of dense stream acid are mixed, will obtain the core-skin composite short fiber and put into this crosslinker solution, be heated to 90 ℃, reacted 2 hours, obtain cross filament;
5. cross filament is immersed and contain dichloroethanes,, rise to 95 ℃ then, reacted 2 hours, obtain described ion-exchange fibre 80 ℃ of reactions 3 hours down by in 2 parts, the sulfonation solution of 98 parts of preparations of the concentrated sulfuric acid.After tested, the exchange capacity of fiber is 3.4mmol/g, and the fiber phenomenon of phase separation is greatly improved.
Embodiment 4:
1. get melt index and be 60 parts of 15 high impact styrenes, melt index is 39.7 parts of 20 polystyrene, crosslinking agent cumyl peroxide (DCP), and 0.3 part, mix after twin-screw, under 235 ℃ of temperature, extrude, granulation, prepare cortex material.
2. getting melt index and be 20 polypropylene is that 20 10 parts of polyethylene, melt index are that 20 high impact polystyrene is 20 parts by 67.9 parts, melt index, bulking agent SB accounts for 2 parts, crosslinking agent cumyl peroxide (DCP) accounts for 0.1 part, after the mixing, under 190 ℃, extrude through twin-screw, the fibre core layered material is prepared in granulation;
3. above-mentioned two kinds of sections are spun out undrawn yarn by 4: 6 core-skins than through core-skin composite spinning silk machine under 275 ℃; Undrawn yarn obtains the core-skin composite short fiber after 100 ℃ of following 3 times of stretchings, oven dry, cut-out after washing;
4,5 with embodiment 3.After tested, the exchange capacity of fiber is 2.3mmol/g, and the fiber phenomenon of phase separation is greatly improved.
Embodiment 5:
1. melt index is 40 parts of 20 high impact styrenes, and melt index is 59.8 parts of 30 polystyrene, crosslinking agent α, and α-(tert-butyl peroxy base) diisopropylbenzene (DIPB), 0.2 part, mix after twin-screw, under 235 ℃ of temperature, extrude, granulation, prepare cortex material;
2. getting melt index and be 30 polypropylene is that 30 polyethylene is that 9 parts, melt index are that 30 high impact polystyrene is 22 parts by 65.8 parts, melt index, bulking agent SBS accounts for 3 parts, crosslinking agent 2,5-dimethyl-2, two (tert-butyl peroxy base) hexanes (AD) of 5-account for 0.2 part, after the mixing, extrude through twin-screw under 190 ℃, the fibre core layered material is prepared in granulation;
With above-mentioned two kinds of sections through core-skin composite spinning silk machine, with 5: 5 core-skin ratios, under 275 ℃, spin out undrawn yarn, undrawn yarn obtains the core-skin composite short fiber after 100 ℃ of following 3 times of stretching, oven dry, cut-out after washing;
4,5. surplus with embodiment 3.After tested, the exchange capacity of fiber is 2.9mmol/g, and the fiber phenomenon of phase separation is greatly improved.
Embodiment 6:
The cross filament that embodiment 5 is obtained immerses the chloromethyl ether that contains catalyst, 45 ℃ down reaction obtain the chloromethylation fiber after 9 hours, again this kind fiber is put into trimethylamine solution, at room temperature react 22 hours after, obtain the strong base ion-exchange fibre.After tested, the exchange capacity of fiber is 3.1mmol/g, and the fiber phenomenon of phase separation is greatly improved.
Embodiment 7:
The chloromethylation fiber that embodiment 6 obtains is put into ethylenediamine solution, obtain weak base type ion-exchange fibre after 13 hours in reaction under 50 ℃.After tested, the exchange capacity of fiber is 3.0mmol/g, and the fiber phenomenon of phase separation is greatly improved.

Claims (6)

1. an ion-exchange fibre is characterized in that this fiber has core-sheath composite structure, and the core-skin weight ratio is 3: 7-7: 3; The percentage by weight prescription of its cortex material is:
High impact polystyrene 20-80%,
Polystyrene 19.5-79.9%,
Crosslinking agent 0.5-0.1%;
The percentage by weight prescription of its core layer material is:
High impact polystyrene 10-30%,
Polypropylene 60.6-74.4%,
Polyethylene 5-15%,
Bulking agent 4-0.5%,
Crosslinking agent 0.4-0.1%;
Wherein, the melt index of high impact polystyrene is 4-30, and the melt index of polystyrene is 5-50, and polyacrylic melt index is 18-50, and poly melt index is 15-60; Described crosslinking agent is 2,5-dimethyl-2, two (tert-butyl peroxy base) hexanes (AD), 2 of 5-, 5-dimethyl-2, two (tert-butyl peroxy base) hexins-3 (YD) of 5-, α, one or more in α-(tert-butyl peroxy base) diisopropylbenzene (DIPB), the cumyl peroxide (DCP); Used crosslinker solution is paraformaldehyde, glacial acetic acid, the concentrated sulfuric acid in 8-2: 25-31 in the fiber cross-linking process: the crosslinker solution of 67 ratios preparation.
2. ion-exchange fibre according to claim 1 is characterized in that the described core-skin weight ratio of this fiber is 4: 6-6: 4.
3. ion-exchange fibre manufacture method according to claim 1 and 2 is characterized in that this method undertaken by following technology:
(1) make the fiber sheath layered material: after high impact styrene, polystyrene, the crosslinking agent of will fill a prescription described melt index and ratio mixes, extrude through twin-screw under 220-260 ℃, granulation produces the fiber sheath layered material;
(2) make the fibre core layered material: after high impact polystyrene, polypropylene, polyethylene, bulking agent, the crosslinking agent of will fill a prescription described melt index and ratio mixes, extrude through twin-screw under 180-230 ℃, granulation produces the fibre core layered material;
(3) make the core-skin composite filament: above-mentioned (1), (2) described cortex material and core layer material are spun out undrawn yarn with core-skin composite spinning silk machine; Undrawn yarn is stretched under 90-110 ℃ of temperature, draw ratio 1.5-3 doubly promptly obtains the core-skin composite filament again;
(4) fiber cross-linking reaction: gained core-skin composite filament put into contain paraformaldehyde, glacial acetic acid, the concentrated sulfuric acid in 8-2: 25-31: the crosslinker solution of 67 ratios preparation 80-95 ℃ of reaction 1.5-3 hour down, obtains cross filament;
(5) fiber functionalization: as required, the gained cross filament is carried out reaction kinetic, can obtain corresponding ion-exchange fibre.
4. ion-exchange fibre manufacture method according to claim 3, it is characterized in that this method described (5) fiber functionalization is a fiber sulfonation treatment process: be about to the gained cross filament and immerse dichloroethanes and the concentrated sulfuric acid in 8-2: in the sulfonated liquid that the 92-98 ratio is prepared, reacted 2-3 hour down at 70-80 ℃, rise to 90-98 ℃ then, reacted 2-3 hour, and can obtain described strong-acid type ion-exchange fibre.
5. ion-exchange fibre manufacture method according to claim 3, it is characterized in that this method described (5) fiber functionalization is the strong amination treatment technology of fiber: be about to the immersion of gained cross filament and contain in the chloromethyl ether solution of catalyst, obtain the chloromethylation fiber in reaction under 45 ℃ after 8-10 hour; Again the gained fiber is put into trimethylamine solution, at room temperature react 20-24 after individual hour, promptly obtain the strong base ion-exchange fibre.
6. ion-exchange fibre manufacture method according to claim 3, it is characterized in that this method described (5) fiber functionalization is the weak amination treatment technology of fiber: be about to the immersion of gained cross filament and contain in the chloromethyl ether solution of catalyst, obtain the chloromethylation fiber in reaction under 45 ℃ after 8-10 hour; Again the gained fiber is put into ethylenediamine solution, promptly obtain weak base type ion-exchange fibre after 12-15 hour in reaction under 50 ℃.
CNB021252041A 2002-07-17 2002-07-17 Ion exchange fibre and its preparing process Expired - Fee Related CN1137000C (en)

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CN103896367B (en) * 2012-12-28 2015-07-22 北京有色金属研究总院 Technology for removing harmful metal ions in beneficiation wastewater by virtue of ion exchange fibers

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