CN104073904A - Method for preparing coarse denier spandex fiber for hygienic material by adopting spandex silk waste - Google Patents
Method for preparing coarse denier spandex fiber for hygienic material by adopting spandex silk waste Download PDFInfo
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Abstract
The invention belongs to the field of material preparation, and relates to a preparation method for coarse denier spandex fiber, in particular to a method for preparing coarse denier spandex fiber for a hygienic material by adopting spandex silk waste. The method comprises the following steps: (1) pre-processing; (2) pre-polymerizing; (3) polymerizing; (4) spinning. In the preparing process of spandex fiber, as the spandex silk waste is treated by a cosolvent, a silicone oil removing additive and a catalyst respectively according to the method, the stable period of a prepared polymer solution is greatly improved, and is longer than 20 days, the fluidity of a polymer stock solution prepared from the spandex silk waste is improved, gelatin in the polymer stock solution is reduced, the spinnability of the polymer stock solution is improved, and the hard segments and the soft segments of the spandex fiber molecular chains obtained by adopting the method are enabled to be structured and ordered.
Description
Technical field
The invention belongs to field of material preparation, relate to the preparation method of thick dawn spandex fibre, be specifically related to a kind of spandex waste silk that utilizes and prepare the method for thick dawn spandex fibre for hygienic material.
Background technology
Spandex is with its good elasticity and Physical Mechanical and be widely used in the fields such as weaving, bio-medical.Rapidly, the output of China's spandex is over 600,000 tons/year in polyurethane fibre industry development in recent years.
Meanwhile, in the production of spandex and use procedure, a large amount of waste silks have also been produced.For these waste silks, take at present the method for burying and burning to process---not only waste a large amount of industrial chemicals, also can cause land wastage and atmosphere pollution, do not met Global Sustainable Development strategy.
Along with the pay attention to day by day of people to environmental issue, the particularly raising of Consciousness of Sustainable Development, eliminate white pollution, realize the reasonable utilization of resource, but because its output only accounts for very little proportion in the extended familys of polyurethane products, therefore the recycling of spandex waste silk was never drawn attention in the past, and the technical barrier that spandex waste silk reclaims is a lot, spandex is linear block polymers of polyurethane, although theoretically, spandex waste silk can carry out secondary dissolving, again make spinning solution, but experiment is found, by spandex waste silk, again make spinning solution stability very poor, mobility also can reduce, very easily generate gel and cannot spinning,
In addition, in the process of spinning for the first time, for the needs of fiber process, surface tends to adhere to the spinning oil that contains the compositions such as amido silicon oil, is convenient to increase the smooth performance of fiber and eliminates the static in procedure of fibre production.But these compositions all can accelerate the degradation speed of spandex waste silk stoste, spandex waste silk polyurethane molecular chain in secondary course of dissolution is ruptured extremely, range of molecular weight distributions is wider, causes its machinability poorer than normal stoste.
The poor stability of spinning solution shows two aspects, one side meeting accelerated degradation, and macromolecular chain destroys serious, reacts too low for apparent viscosity, in polymer dope spinning process, can, from spinneret orifice and spinning shaft Fracture, be difficult to continuous machine-shaping; In addition, part group can carry out cross-linking reaction, and generation can not be dissolved in the gel particle in system, and these particles have elasticity, in spinning process process, under certain pressure effect, can pass through filter, enter in the spinneret component of spinning, while passing through the spinneret orifice of spinnerets, spinneret orifice can be stopped up, cause polymer dope cutout, be difficult to equally continuous machine-shaping.
Summary of the invention
Goal of the invention: the problem that the present invention is directed to above-mentioned prior art existence makes improvements, and the invention provides a kind of spandex waste silk that utilizes and prepares the method for thick dawn spandex fibre for hygienic material.
Technical scheme: a kind of spandex waste silk that utilizes is prepared the method for thick dawn spandex fibre for hygienic material, and its step comprises:
(1), preliminary treatment:
(11) spandex waste silk is sorted to also impurities removing;
(12) the described spandex waste silk after step (11) sorting is organized into waste silk bundle;
(13) the described waste silk bundle of step (12) is switched to the staple fibre of 3～10cm;
(14) according to volume ratio water: desiliconization oil assistant=100:(1～5) configuration cleaning fluid, the described staple fibre of step (13) is cleaned to 30～80min with described cleaning fluid, the mass ratio of described staple fibre and described cleaning fluid is 1:5～1:20;
(15) staple fibre after the described cleaning of step (14) being dried to extremely moisture mass percent is 0.01%～2%;
(2), prepolymerization: according to the ratio of 1～5 part of 10～45 parts, spandex waste silk staple fibre, 55～90 parts of polar solvents and cosolvent, spandex waste silk staple fibre step (15) Suo Shu is dropped into reaction kettle for reaction and form prepolymerization product, reaction temperature is 35～40 ℃, and the reaction time is 30～60min;
(3), polymerization: first add catalyst in the described prepolymerization product of step (2), the consumption of described catalyst is 1%～5% of described prepolymerization product quality; Described prepolymerization product is transplanted on to polymerization in polymerization reaction kettle again and forms polymer dope, the reaction temperature of polymerisation is 30～80 ℃, and the reaction time of polymerisation is 150～180min;
(4), spinning: the polymer dope that step (3) is made adopts dry-spinning silk method to make thick dawn spandex fibre for hygienic material.
As utilizing spandex waste silk in the present invention, prepare a kind of preferred version of the method for thick dawn spandex fibre for hygienic material: the described desiliconization oil assistant of step (14) component is: 77.5 parts of 8～12 parts of DDAOs, 3～5 parts of modification cocoanut fatty acid diethanolamides, 2～4 parts of sodium xylene sulfonates, EDTA5～8 part and deionized waters.
As utilizing spandex waste silk in the present invention, prepare a kind of preferred version of the method for thick dawn spandex fibre for hygienic material: the described desiliconization oil assistant of step (14) component is: 77.5 parts of 8～12 parts of DDAOs, 3～5 parts of modification cocoanut fatty acid diethanolamides, 2～4 parts of sodium xylene sulfonates, NTA5～8 part and deionized waters.
As utilizing spandex waste silk in the present invention, prepare a kind of preferred version of the method for thick dawn spandex fibre for hygienic material: the described cosolvent of step (2) is one or more in urethanes, urea, formamide, acetamide.
As utilizing spandex waste silk in the present invention, prepare a kind of preferred version of the method for thick dawn spandex fibre for hygienic material: described in step (2), polar solvent is one or more in DMAc, DMF, DMSO, NMP.
As utilizing spandex waste silk in the present invention, prepare a kind of preferred version of the method for thick dawn spandex fibre for hygienic material: the described prepolymerization product of step (2) apparent viscosity at 20 ℃ is 2000～8000poise.
As utilizing spandex waste silk in the present invention, prepare a kind of preferred version of the method for thick dawn spandex fibre for hygienic material: the described catalyst of step (3) be dibutyl tin dilaurate, stannous octoate one or both.
As utilizing spandex waste silk in the present invention, prepare a kind of preferred version of the method for thick dawn spandex fibre for hygienic material: the described polymer dope of step (3) is 3000～12000poise the apparent viscosity of 20 ℃.
As utilizing spandex waste silk in the present invention, prepare a kind of preferred version of the method for thick dawn spandex fibre for hygienic material: in step (4), the technological parameter of dry spin processes is: spinning head temperature is 210～300 ℃, and spinning speed is 300～750m/min.
As utilizing spandex waste silk in the present invention, prepare a kind of preferred version of the method for thick dawn spandex fibre for hygienic material: described in step (1), baking temperature is 120～250 ℃, and be 180～260min drying time.
Beneficial effect: in the process that 1, the present invention is dissolved at spandex waste silk secondary, in conjunction with chemical method, adopt cosolvent, desiliconization oil assistant and catalyst, greatly improved the stationary phase of prepared polymer dope (being greater than 20 days);
2, for the shortcoming of waste silk stoste poor fluidity, the present invention, by adding the mode of cosolvent, makes the sex change of waste silk stoste in polymerization process, improves its mobility, reduces the gel in polymer dope, has improved the spinnability of polymer dope.The polymer solids level obtaining after polymerisation is controlled at 10%～45%, and polymer dope apparent viscosity is 3000～12000poise in the time of 20 ℃, makes it meet the requirement of spinning process completely;
3, the spandex fibre that method of the present invention obtains and the character of conventional spandex fibre have bigger difference, although soft section of part of macromolecular main chain is identical with conventional spandex, but make in strand hard section more regular in order by adding the additives such as cosolvent, catalyst, desiliconization oil assistant, polymer dope stability, rheological characteristic, processability have been improved, guarantee that soft section larger deformation easily occurs under effect of stress, fiber has lower modulus, thereby gives the characteristic of the good low stress of fiber.
The specific embodiment:
Below the specific embodiment of the present invention is described in detail.
Specific embodiment 1
Utilize spandex waste silk to prepare a method for thick dawn spandex fibre for hygienic material, its step comprises:
(1), preliminary treatment:
(11) spandex waste silk is sorted to also impurities removing;
(12) spandex waste silk after step (11) sorting is organized into waste silk bundle (waste silk is entwined in the same way);
(13) step (12) spandex bundle is switched to the staple fibre of 3cm left and right;
(14) according to volume ratio water: desiliconization oil assistant=100:5 configures cleaning fluid, the staple fibre of step (13) is cleaned to 30min with cleaning fluid, the mass ratio of staple fibre and cleaning fluid is 1:5;
(15) staple fibre after cleaning in step (14) being dried to extremely moisture mass percent is 0.01%, and baking temperature is 250 ℃, and be 260min drying time;
(2), prepolymerization: according to the ratio of 1 part of 10 parts, spandex waste silk staple fibre, 90 parts of DMAc (polar solvent) and urethanes (cosolvent), the spandex waste silk staple fibre of step (15) is dropped into reaction kettle for reaction and form prepolymerization product, reaction temperature is 35 ℃, reaction time is 60min, and prepolymerization product apparent viscosity at 20 ℃ is 8000poise;
(3), polymerization: first in step (2) prepolymerization product, add dibutyl tin dilaurate (catalyst), the consumption of dibutyl tin dilaurate be prepolymerization product quality 1%; Again prepolymerization product (with catalyst) is transplanted on to polymerization in polymerization reaction kettle and forms polymer dope, the reaction temperature of polymerisation is 30 ℃, the reaction time of polymerisation is 180min, and the apparent viscosity of polymer dope is 12000poise at 20 ℃;
(4), spinning: the polymer dope that step (3) is made adopts dry-spinning silk method to make thick dawn spandex fibre for hygienic material, and technological parameter is: spinning head temperature is 300 ℃, and spinning speed is 750m/min.
Step (14) desiliconization oil assistant component is: 77.5 parts of 8 parts of DDAOs, 3 parts of modification cocoanut fatty acid diethanolamides, 2 parts of sodium xylene sulfonates, EDTA5 part and deionized waters.
Specific embodiment 2
Utilize spandex waste silk to prepare a method for thick dawn spandex fibre for hygienic material, its step comprises:
(1), preliminary treatment:
(11) spandex waste silk is sorted to also impurities removing;
(12) spandex waste silk after step (11) sorting is organized into waste silk bundle (waste silk is entwined in the same way);
(13) step (12) spandex bundle is switched to the staple fibre of 10cm left and right;
(14) according to volume ratio water: desiliconization oil assistant=100:1 configures cleaning fluid, step (13) staple fibre is cleaned to 80min with cleaning fluid, the mass ratio of staple fibre and cleaning fluid is 1:10;
(15) staple fibre after cleaning in step (14) being dried to extremely moisture mass percent is 2%, and baking temperature is 120 ℃, is about 180min drying time;
(2), prepolymerization: according to the ratio of 5 parts, 45 parts, spandex waste silk staple fibre, 55 parts of DMF (polar solvent) and urea (cosolvent), the spandex waste silk staple fibre of step (15) is dropped into reaction kettle for reaction and form prepolymerization product, reaction temperature is 40 ℃, reaction time is 30min, and prepolymerization product apparent viscosity at 20 ℃ is 2000poise;
(3), polymerization: first in step (2) prepolymerization product, add stannous octoate (catalyst), the consumption of stannous octoate be prepolymerization product quality 5%; Prepolymerization product (with catalyst) is transplanted on to polymerization in polymerization reaction kettle again and forms polymer dope, the reaction temperature of polymerisation is 80 ℃, and the reaction time of polymerisation is 150min, and the apparent viscosity of polymer dope is 3000poise at 20 ℃;
(4), spinning: the polymer dope that step (3) is made adopts dry-spinning silk method to make thick dawn spandex fibre for hygienic material, and technological parameter is: spinning head temperature is 210 ℃, and spinning speed is 300m/min.
Step (14) desiliconization oil assistant component is: 77.5 parts of 12 parts of DDAOs, 5 parts of modification cocoanut fatty acid diethanolamides, 4 parts of sodium xylene sulfonates, EDTA5 part and deionized waters.
Specific embodiment 3
Utilize spandex waste silk to prepare a method for thick dawn spandex fibre for hygienic material, its step comprises:
(1), preliminary treatment:
(11) spandex waste silk is sorted to also impurities removing;
(12) spandex waste silk after step (11) sorting is organized into waste silk bundle (waste silk is entwined in the same way);
(13) step (12) spandex bundle is switched to the staple fibre of 5cm left and right;
(14) according to volume ratio water: desiliconization oil assistant=100:3 configures cleaning fluid, the staple fibre of step (13) is cleaned to 50min with cleaning fluid, the mass ratio of staple fibre and cleaning fluid is 1:20;
(15) staple fibre after cleaning in step (14) being dried to extremely moisture mass percent is 1%, and baking temperature is 150 ℃, is about 200min drying time;
(2), prepolymerization: according to the ratio of 3 parts of 30 parts, spandex waste silk staple fibre, 70 parts of DMSO (polar solvent) and formamides (cosolvent), the spandex waste silk staple fibre of step (15) is dropped into reaction kettle for reaction and form prepolymerization product, reaction temperature is 38 ℃, reaction time is 45min, and prepolymerization product apparent viscosity at 20 ℃ is 5000poise;
(3), polymerization: first in step (2) prepolymerization product, add stannous octoate (catalyst), the consumption of stannous octoate be prepolymerization product quality 3%; Prepolymerization product (with catalyst) is transplanted on to polymerization in polymerization reaction kettle again and forms polymer dope, the reaction temperature of polymerisation is 50 ℃, and the reaction time of polymerisation is 165min, and the apparent viscosity of polymer dope is 6000poise at 20 ℃;
(4), spinning: the polymer dope that step (3) is made adopts dry-spinning silk method to make thick dawn spandex fibre for hygienic material, and technological parameter is: spinning head temperature is 250 ℃, and spinning speed is 450m/min.
Step (14) desiliconization oil assistant component is: 77.5 parts of 10 parts of DDAOs, 4 parts of modification cocoanut fatty acid diethanolamides, 3 parts of sodium xylene sulfonates, EDTA6 part and deionized waters.
Specific embodiment 4
Roughly the same with concrete enforcement 1, difference is only:
1, the polar solvent in step (2) is NMP, and cosolvent is acetamide;
2, step (14) desiliconization oil assistant component is: 77.5 parts of 8 parts of DDAOs, 3 parts of modification cocoanut fatty acid diethanolamides, 2 parts of sodium xylene sulfonates, NTA5 part and deionized waters.
Specific embodiment 5
Roughly the same with concrete enforcement 1, difference is only:
1, the polar solvent in step (2) is NMP and DMF, its mass ratio 1:1 (its ratio can be allocated arbitrarily);
2, the cosolvent in step (2) is urethanes and urea, its mass ratio 1:1 (its ratio can be allocated arbitrarily);
3, step (14) desiliconization oil assistant component is: 77.5 parts of 12 parts of DDAOs, 5 parts of modification cocoanut fatty acid diethanolamides, 4 parts of sodium xylene sulfonates, NTA5 part and deionized waters.
Specific embodiment 6
Roughly the same with concrete enforcement 1, difference is only:
1, the polar solvent in step (2) is NMP and DMSO, its mass ratio 1:1 (its ratio can be allocated arbitrarily);
2, the cosolvent in step (2) is urethanes and formamide, its mass ratio 1:1 (its ratio can be allocated arbitrarily);
3, step (14) desiliconization oil assistant component is: 77.5 parts of 10 parts of DDAOs, 4 parts of modification cocoanut fatty acid diethanolamides, 3 parts of sodium xylene sulfonates, EDTA6 part and deionized waters.
Specific embodiment 7
Roughly the same with concrete enforcement 1, difference is only:
1, the polar solvent in step (2) is NMP and DMAc, its mass ratio 1:1 (its ratio can be allocated arbitrarily);
2, the cosolvent in step (2) is urethanes and acetamide, its mass ratio 1:1 (its ratio can be allocated arbitrarily).
Specific embodiment 8
Roughly the same with concrete enforcement 1, difference is only:
1, the polar solvent in step (2) such as is at DMAc, DMF, DMSO, the NMP (its ratio can be allocated arbitrarily) of mass ratio;
3, the cosolvent in step (2) such as is at urethanes, urea, formamide, the acetamide (its ratio can be allocated arbitrarily) of mass ratio.
The compositions of mixtures of explaining according to umber in specific embodiment is all mass fraction in the situation that not specializing.For example 10～45 parts, spandex waste silk staple fibre, 55～90 parts of polar solvents and cosolvent are 1～5 part, all refer to mass fraction in the situation that specifically not indicating.
Above embodiments of the present invention are described in detail.But the present invention is not limited to above-mentioned embodiment, in the ken possessing at affiliated technical field those of ordinary skill, can also under the prerequisite that does not depart from aim of the present invention, make a variety of changes.
Claims (10)
1. utilize spandex waste silk to prepare a method for thick dawn spandex fibre for hygienic material, comprise the following steps:
(1), preliminary treatment:
(11) spandex waste silk is sorted to also impurities removing;
(12) the described spandex waste silk after step (11) sorting is organized into waste silk bundle;
(13) the described waste silk bundle of step (12) is switched to the staple fibre of 3～10cm;
(14) according to volume ratio water: desiliconization oil assistant=100:(1～5) configuration cleaning fluid, the described staple fibre of step (13) is cleaned to 30～80min with described cleaning fluid, the mass ratio of described staple fibre and described cleaning fluid is 1:5～1:20;
(15) staple fibre after the described cleaning of step (14) being dried to extremely moisture mass percent is 0.01%～2%;
(2), prepolymerization: according to the ratio of 1～5 part of 10～45 parts, spandex waste silk staple fibre, 55～90 parts of polar solvents and cosolvent, spandex waste silk staple fibre step (15) Suo Shu is dropped into reaction kettle for reaction and form prepolymerization product, reaction temperature is 35～40 ℃, and the reaction time is 30～60min;
(3), polymerization: first in the described prepolymerization product of step (2), add catalyst, the consumption of described catalyst be described prepolymerization product quality 1%～5%; Described prepolymerization product is transplanted on to polymerization in polymerization reaction kettle again and forms polymer dope, the reaction temperature of polymerisation is 30～80 ℃, and the reaction time of polymerisation is 150～180min;
(4), spinning: the polymer dope that step (3) is made adopts dry-spinning silk method to make thick dawn spandex fibre for hygienic material.
2. the spandex waste silk that utilizes as claimed in claim 1 is prepared the method for thick dawn spandex fibre for hygienic material, it is characterized in that, the described desiliconization oil assistant of step (14) component is: 77.5 parts of 8～12 parts of DDAOs, 3～5 parts of modification cocoanut fatty acid diethanolamides, 2～4 parts of sodium xylene sulfonates, EDTA5～8 part and deionized waters.
3. the spandex waste silk that utilizes as claimed in claim 1 is prepared the method for thick dawn spandex fibre for hygienic material, it is characterized in that, the described desiliconization oil assistant of step (14) component is: 77.5 parts of 8～12 parts of DDAOs, 3～5 parts of modification cocoanut fatty acid diethanolamides, 2～4 parts of sodium xylene sulfonates, NTA5～8 part and deionized waters.
4. the spandex waste silk that utilizes as claimed in claim 1 is prepared the method for thick dawn spandex fibre for hygienic material, it is characterized in that, the described cosolvent of step (2) is one or more in urethanes, urea, formamide, acetamide.
5. the spandex waste silk that utilizes as claimed in claim 1 is prepared the method for thick dawn spandex fibre for hygienic material, it is characterized in that, described in step (2), polar solvent is one or more in DMAc, DMF, DMSO, NMP.
6. the spandex waste silk that utilizes as claimed in claim 1 is prepared the method for thick dawn spandex fibre for hygienic material, it is characterized in that, the described prepolymerization product of step (2) apparent viscosity at 20 ℃ is 2000～8000poise.
7. the spandex waste silk that utilizes as claimed in claim 1 is prepared the method for thick dawn spandex fibre for hygienic material, it is characterized in that, the described catalyst of step (3) be dibutyl tin dilaurate, stannous octoate one or both.
8. the spandex waste silk that utilizes as claimed in claim 1 is prepared the method for thick dawn spandex fibre for hygienic material, it is characterized in that, the apparent viscosity that the described polymer dope of step (3) is 20 ℃ is 3000～12000poise.
9. the spandex waste silk that utilizes as claimed in claim 1 is prepared the method for thick dawn spandex fibre for hygienic material, it is characterized in that, the technological parameter in step (4) is: spinning head temperature is 210～300 ℃, and spinning speed is 300～750m/min.
10. the spandex waste silk that utilizes as claimed in claim 1 is prepared the method for thick dawn spandex fibre for hygienic material, it is characterized in that, described in step (1), baking temperature is 120～250 ℃, and be 180～260min drying time.
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| CN107099873A (en) * | 2017-06-15 | 2017-08-29 | 淮安侨新新材料科技有限公司 | Spandex waste silk regenerates the preparation method of false proof spandex fibre |
| CN110885538A (en) * | 2019-12-08 | 2020-03-17 | 周佩珍 | Flame-retardant high-temperature-resistant electric wire and manufacturing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107099873A (en) * | 2017-06-15 | 2017-08-29 | 淮安侨新新材料科技有限公司 | Spandex waste silk regenerates the preparation method of false proof spandex fibre |
| CN110885538A (en) * | 2019-12-08 | 2020-03-17 | 周佩珍 | Flame-retardant high-temperature-resistant electric wire and manufacturing method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104073904B (en) | 2016-01-20 |
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